Crystal structures and hydrogen bonding in the isotypic series of hydrated alkali metal (K, Rb and Cs) complexes with 4-amino­phenyl­arsonic acid

Smith, G.; Wermuth, U.D.

doi:10.1107/S2056989017000445

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Volume 73| Part 2| February 2017| Pages 203-208

https://doi.org/10.1107/S2056989017000445

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Crystal structures and hydrogen bonding in the isotypic series of hydrated alkali metal (K, Rb and Cs) complexes with 4-aminophenylarsonic acid

Graham Smith ^a ^* and Urs D. Wermuth ^b

^aScience and Engineering Faculty, Queensland University of Technology, GPO Box 2434, Brisbane, Queensland 4001, Australia, and ^bSchool of Natural Sciences, Griffith University, Nathan, Queensland 4111, Australia
^*Correspondence e-mail: gsmith@bigpond.com

Edited by M. Weil, Vienna University of Technology, Austria (Received 7 December 2016; accepted 10 January 2017; online 17 January 2017)

The structures of the alkali metal (K, Rb and Cs) complex salts with 4-aminophenylarsonic acid (p-arsanilic acid) manifest an isotypic series with the general formula [M₂(C₆H₇AsNO₃)₂(H₂O)₃], with M = K {poly[di-μ₃-4-aminophenylarsonato-tri-μ₂-aqua-dipotassium], [K₂(C₆H₇AsNO₃)₂(H₂O)₃], (I)}, Rb {poly[di-μ₃-4-aminophenylarsonato-tri-μ₂-aqua-dirubidium], [Rb₂(C₆H₇AsNO₃)₂(H₂O)₃], (II)}, and Cs {poly[di-μ₃-4-aminophenylarsonato-tri-μ₂-aqua-dirubidium], [Cs₂(C₆H₇AsNO₃)₂(H₂O)₃], (III)}, in which the repeating structural units lie across crystallographic mirror planes containing two independent and different metal cations and a bridging water molecule, with the two hydrogen p-arsanilate ligands and the second water molecule lying outside the mirror plane. The bonding about the two metal cations in all complexes is similar, one five-coordinate, the other progressing from five-coordinate in (I) to eight-coordinate in both (II) and (III), with overall M—O bond-length ranges of 2.694 (5)–3.009 (7) (K), 2.818 (4)–3.246 (4) (Rb) and 2.961 (9)–3.400 (10) Å (Cs). The additional three bonds in (II) and (III) are the result of inter-metal bridging through the water ligands. Two-dimensional coordination polymeric structures with the layers lying parallel to (100) are generated through a number of bridging bonds involving the water molecules (including hydrogen-bonding interactions), as well as through the arsanilate O atoms. These layers are linked across [100] through amine N—H⋯O hydrogen bonds to arsonate and water O-atom acceptors, giving overall three-dimensional network structures.

Keywords: crystal structure; p-arsanilic acid; coordination polymers; alkali metal salts; hydrogen bonding.

CCDC references: 1526425; 1526424; 1526423

1. Chemical context

Arsenical 4-aminophenylarsonic acid (p-arsanilic acid) has biological significance as an anti-helminth in veterinary applications (Steverding, 2010 ; O'Neil, 2001 ) and as a hydrated sodium salt (atoxyl) that had early usage as an anti-syphilitic (Ehrlich & Bertheim, 1907 ; Bosch & Rosich, 2008 ). The crystal structure of this salt has been determined together with the NH₄⁺ salt (Smith & Wermuth, 2014 ); the structure of the parent p-arsanilic acid, which exists as a zwitterion, is also known (Shimada, 1961 ; Nuttall & Hunter, 1996 ). We have also determined the structures of the alkaline earth metal (Mg, Ca, Sr, Ba) salts of the acid (Smith & Wermuth, 2017 ). However, simple p-arsanilate single-metal complex structures are not common in the Cambridge Structure Database (Groom et al., 2016 ), examples being with Ag^I (three forms), Zn, Pb and Cd (Lesikar-Parrish et al., 2013 ; Xiao et al., 2015 ); Zn (Lin et al., 2012 ); Cd (Liu et al., 2010 ); Sn^IV (Xie et al., 2008 ); V^IV and V^V (Breen et al., 2012 ; Chen et al., 2012 ; Khan et al., 1992 ); UO₂ (Adelani et al., 2012 ). Mixed-metal and/or mixed-ligand complexes are common, e.g. Co^II/Mo=O, Ni^II/Mo=O, Cu^II/Mo=O and Zn/Mo=O with p-arsanilate and ligands such as 2,2′-bipyridine, 4,4′-bipyridine and 1,10-phenanthroline (Smith et al., 2013 ).

In an attempt to complete the structures of the alkali metal series of p-arsanilate salts, our reaction of the acid with potassium carbonate, rubidium carbonate and caesium carbonate in ethanol/water resulted in the formation of the crystalline hydrated salts with general formula [M⁺₂(C₆H₇AsNO₃)⁻₂·3H₂O]. Compounds (I) (M = K), (II) (Rb) and (III) (Cs) and their crystal structures are reported herein. However, suitable crystals of the Li analogue were not obtained to allow its crystal structure determination.

2. Structural commentary

The structures of the three title compounds [(I), (II) and (III)] form an isotypic series, with the asymmetric units in each comprising two independent and different metal complex cations (M1 and M2), which lie on crystallographic mirror planes that also contain one of the coordinating water molecules (O2W), with the hydrogen p-arsanilate ligands and the second water molecules (OW1, O1Wⁱⁱ) [symmetry code: (ii) −x + 1, −y, z] lying across the mirror plane (Figs. 1, 2 and 3, respectively). In all three examples, the M2 cation is five-coordinate, while with M1, the coordination spheres progress from five-coordinate in (I) to eight-coordinate in (II) and (III). The overall M—O bond length ranges are 2.694 (5)–3.009 (7) Å (K) (Table 1), 2.818 (4)–3.246 (4) Å (Rb) (Table 2) and 2.961 (9)–3.400 (10) Å (Cs) (Table 2). The amine N atom is not involved in bonding to the metal, as is the case in a number of other p-arsanilate complexes, e.g. with Zn (Lin et al., 2012). The M1O₅ polyhedra in all three structures comprise four bridging arsonate O atoms and the μ₂ bridging water molecule (O2W) (Tables 1, 2 and 3). The second M2O₅ polyhedron in (I) comprises the bridging O11 and O11ⁱⁱ donors, the μ₂-O2Wⁱ [symmetry code: (i) −x + 1, −y + 2, z + $[{1\over 2}]$ ] donor and two monodentate water molecules (O1W and O1Wⁱ) (Table 1).

Table 1
Selected bond lengths (Å) for (I)

K1—O1W	2.766 (5)	K2—O2W	3.009 (7)
K1—O11	2.824 (4)	K2—O11	2.713 (5)
K1—O2Wⁱ	2.959 (7)	K2—O12ⁱⁱⁱ	2.694 (5)
K1—O1Wⁱⁱ	2.766 (5)	K2—O11ⁱⁱ	2.713 (5)
K1—O11ⁱⁱ	2.824 (4)	K2—O12^iv	2.694 (5)
Symmetry codes: (i) $[-x+1, -y+2, z+{\script{1\over 2}}]$ ; (ii) -x+1, y, z; (iii) $[-x+1, -y+1, z-{\script{1\over 2}}]$ ; (iv) $[x, -y+1, z-{\script{1\over 2}}]$ .

Table 2
Selected bond lengths (Å) for (II)

Rb1—O1W	2.917 (4)	Rb1—O1W^v	3.246 (4)
Rb1—O11	2.925 (3)	Rb2—O2W	3.193 (6)
Rb1—O2Wⁱ	3.151 (6)	Rb2—O11	2.863 (3)
Rb1—O1Wⁱⁱ	3.246 (4)	Rb2—O12^vi	2.818 (4)
Rb1—O2Wⁱⁱⁱ	3.109 (5)	Rb2—O11^iv	2.863 (3)
Rb1—O1W^iv	2.917 (4)	Rb2—O12^vii	2.818 (4)
Rb1—O11^iv	2.925 (3)
Symmetry codes: (i) x, y, z+1; (ii) $[-x+1, -y+2, z-{\script{1\over 2}}]$ ; (iii) $[-x+1, -y+2, z+{\script{1\over 2}}]$ ; (iv) -x+1, y, z; (v) $[x, -y+2, z-{\script{1\over 2}}]$ ; (vi) $[-x+1, -y+1, z-{\script{1\over 2}}]$ ; (vii) $[x, -y+1, z-{\script{1\over 2}}]$ .

Table 3
Selected bond lengths (Å) for (III)

Cs1—O1W	3.087 (9)	Cs1—O1Wⁱⁱⁱ	3.400 (10)
Cs1—O2W	3.286 (13)	Cs2—O11	3.024 (8)
Cs1—O11	3.040 (8)	Cs2—O2W^iv	3.324 (13)
Cs1—O1Wⁱ	3.400 (10)	Cs2—O12^v	2.961 (9)
Cs1—O2Wⁱ	3.295 (12)	Cs2—O11ⁱⁱ	3.024 (8)
Cs1—O1Wⁱⁱ	3.087 (9)	Cs2—O12^vi	2.961 (9)
Cs1—O11ⁱⁱ	3.040 (8)
Symmetry codes: (i) $[-x+1, -y+2, z+{\script{1\over 2}}]$ ; (ii) -x+1, y, z; (iii) $[x, -y+2, z+{\script{1\over 2}}]$ ; (iv) x, y, z+1; (v) $[-x+1, -y+1, z+{\script{1\over 2}}]$ ; (vi) $[x, -y+1, z+{\script{1\over 2}}]$ .

Figure 1
The molecular configuration and atom numbering scheme for the complex unit in (I)

. The metal cations (K1 and K2) and the water molecule (O2W) lie on a mirror plane with mirror-related atoms indicated by symmetry code (ii) −x + 1, −y, z + $[{1\over 2}]$ . For other codes, see Table 1

. Non-H atoms are shown as displacement ellipsoids at the 40% probability level.

Figure 2
The molecular configuration and atom numbering scheme for the complex unit in the isotypic structure (II)

. The metal cations (Rb1 and Rb2) and the water molecule (O2W) also lie on a mirror plane. For symmetry codes, see Table 2

. Non-H atoms are shown as displacement ellipsoids at the 40% probability level.

Figure 3
The molecular configuration and atom numbering scheme for the complex unit in the isotypic structure (III)

. The metal cations (Cs1 and Cs2) and the water molecule (O2W) also lie on a mirror plane. For symmetry codes, see Table 3

. Non-H atoms are shown as displacement ellipsoids at the 40% probability level.

With (II) and (III), the irregular M2O₈ coordination sphere comprises all bonds mentioned in the description of the K complex (I), and in addition, the Rb and Cs bond length expansion allows further coordination sites through additional bridging bonds to both of the water molecules (two through O1W and one through O2W), (Tables 2 and 3). The M1⋯M2 separations are 4.139 (3) Å [for (I)], 4.2500 (11) Å [for (II)] and 4.3498 (15) Å [for (III)]. There are also slightly shorter M1⋯M1ⁱ separations in all structures: 4.079 (3) Å (I), 4.1953 (13) Å (II) and 4.3127 (16) Å (III). Relatively short M2⋯As1 separations are present within the repeat unit in all three structures: 3.6369 (19) Å (I), 3.7796 (8) Å (II) and 3.9488 (14) Å (III).

In all structures, two-dimensional coordination polymeric complex structures are generated, with the layers lying in the mirror planes parallel to (100). Fig. 4 shows the basic makeup of the layer in (I) while those for (II) or (III) are shown in Fig. 5. The water molecule O2W provides hydrogen-bonding links across the mirror plane to arsonate O13 acceptors (Tables 4, 5 and 6).

Table 4
Hydrogen-bond geometry (Å, °) for (I)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H11W⋯N4^v	0.88 (6)	2.05 (6)	2.915 (7)	171 (5)
O1W—H12W⋯O11^vi	0.89 (5)	1.77 (5)	2.660 (6)	175 (7)
O2W—H21W⋯O13^vii	0.86 (5)	2.09 (6)	2.819 (6)	142 (6)
O12—H12⋯O13^iv	0.87 (6)	1.70 (6)	2.538 (7)	160 (7)
N4—H41⋯O1W^viii	0.86 (5)	2.17 (5)	3.010 (7)	164 (5)
N4—H42⋯O13^ix	0.87 (6)	2.15 (6)	2.984 (7)	160 (5)
Symmetry codes: (iv) $[x, -y+1, z-{\script{1\over 2}}]$ ; (v) $[-x+{\script{3\over 2}}, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ ; (vi) $[x, -y+2, z+{\script{1\over 2}}]$ ; (vii) x, y, z-1; (viii) $[-x+{\script{3\over 2}}, y-{\script{1\over 2}}, z]$ ; (ix) $[-x+{\script{3\over 2}}, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ .

Table 5
Hydrogen-bond geometry (Å, °) for (II)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H11W⋯N4^viii	0.89 (5)	2.04 (4)	2.923 (6)	176 (5)
O2W—H21W⋯O13^ix	0.88 (4)	1.97 (4)	2.852 (5)	173 (5)
O12—H12⋯O13^vii	0.86 (3)	1.73 (4)	2.552 (5)	158 (5)
N4—H41⋯O13^x	0.86 (5)	2.18 (4)	3.022 (5)	167 (4)
N4—H42⋯O1W^xi	0.88 (4)	2.13 (4)	3.005 (6)	176 (4)
Symmetry codes: (vii) $[x, -y+1, z-{\script{1\over 2}}]$ ; (viii) $[-x+{\script{3\over 2}}, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ ; (ix) x, y, z-1; (x) $[-x+{\script{3\over 2}}, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (xi) $[-x+{\script{3\over 2}}, y-{\script{1\over 2}}, z]$ .

Table 6
Hydrogen-bond geometry (Å, °) for (III)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H11W⋯N4^vii	0.89 (9)	2.28 (13)	2.952 (13)	132 (10)
O2W—H21W⋯O13	0.89 (12)	2.16 (12)	2.850 (10)	134 (12)
O12—H12⋯O13^vi	0.88 (5)	2.00 (12)	2.567 (13)	121 (12)
N4—H41⋯O1W^viii	0.83 (14)	2.12 (15)	2.928 (15)	164 (9)
N4—H42⋯O13^ix	0.91 (14)	2.20 (14)	3.082 (13)	166 (15)
Symmetry codes: (vi) $[x, -y+1, z+{\script{1\over 2}}]$ ; (vii) $[-x+{\script{3\over 2}}, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (viii) $[-x+{\script{3\over 2}}, y-{\script{1\over 2}}, z]$ ; (ix) $[-x+{\script{3\over 2}}, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ .

Figure 4
A partial expansion of the two-dimensional coordination polymeric sheet structure of (I)

, which extends across the mirror plane parallel to (100). Aromatic H atoms are omitted. For symmetry codes, see Table 1

Figure 5
A partial expansion of the two-dimensional coordination polymeric sheet structure of (II)

[or (III)], which extends across the mirror plane parallel to (100). Aromatic H atoms have been omitted.

3. Supramolecular features

In the crystals of all three compounds, similar overall packing modes are observed, with the coordination polymeric layers lying along the mirror planes inter-linked across [100] through amine N4—H⋯O hydrogen bonds to arsonate O13 and water O1W acceptors (Tables 4, 5 and 6). In this respect, they resemble the crystal packing of the Na p-arsanilate analogue (Smith & Wermuth, 2014) but the structure of that compound (a trihydrate) differs from the current isotypic set in having significantly different coordination spheres, also lacking the mirror symmetry of the primary polymeric layers in (I)–(III). With these, the N4 amino group acts as an acceptor to an O1W hydrogen bond. The water molecule O1W also forms a hydrogen bond with O11^vi [symmetry code: (vi) x, −y + 2, z + $[{1\over 2}]$ ] in (I), but not in (II) or (III). The protonated p-arsanilate O atom (O12) forms an intra-layer hydrogen bond with an O11 acceptor, giving overall three-dimensional network structures in all cases (Figs. 6 and 7). No π–π associations are present in the structures.

Figure 6
A view of the packing in the unit cell of (I)

along [010], showing the associated cation/anion sheets linked peripherally across [100] by hydrogen bonds involving the anilinium amine groups. Hydrogen-bonding interactions are shown as dashed lines and aromatic H atoms have been omitted.

Figure 7
A view of the packing in the unit cell of (II)

[or (III)] along [010], showing the associated cation/anion sheets linked peripherally across [100] by hydrogen bonds involving the amine groups.

4. Database survey

Three-dimensional supramolecular structures involving complexes of hydrogen p-arsanilate and mixed metal types, as distinct from those involving uni-metal types, such as in (I)–(III) and in those examples which have been previously mentioned in the Chemical context section of this article, are worthy of noting here. Mixed-metal-ligand examples (Smith et al., 2013) as well as mixed–metal structures add to the complexity of the coordination polymeric structures commonly generated, e.g. in the Mo/Ag, Mo/Cu and W/Na polyoxidometallate compounds (Johnson et al., 2002 ), the Mo/V cage structure (Onet et al., 2011 ) or the V/Na structure (Breen & Schmitt, 2008 ).

5. Synthesis and crystallization

Compounds (I)–(III) were synthesized by heating together for 5 min, 1 mmol quantities of 4-aminophenylarsonic acid and 0.5 mmol of either K₂CO₃ [for (I)], Rb₂CO₃ [for (II)] or Cs₂CO₃ [for (III)], in 20 ml of 50% ethanol/water (v/v). Room temperature evaporation of the solutions gave colourless crystal plates of the title compounds from which specimens were cleaved for the X-ray analyses.

6. Refinement details

Crystal data, data collection and structure refinement details are summarized in Table 7. Hydrogen atoms potentially involved in hydrogen-bonding interactions were located by difference methods but their positional parameters were restrained in the refinement with N—H = 0.88 Å and O—H = 0.86 Å, and with U_iso(H) = 1.2U_eq(N) or 1.5U_eq(O). Other H atoms were included in the refinement at calculated positions, C—H = 0.95 Å, and treated as riding with U_iso(H) = 1.2U_eq(C).

Table 7
Experimental details

	(I)	(II)	(III)
Crystal data
Chemical formula	[K₂(C₆H₇AsNO₃)₂(H₂O)₃]	[Rb₂(C₆H₇AsNO₃)₂(H₂O)₃]	[Cs₂(C₆H₇AsNO₃)₂(H₂O)₃]
M_r	564.34	657.08	751.96
Crystal system, space group	Orthorhombic, Cmc2₁	Orthorhombic, Cmc2₁	Orthorhombic, Cmc2₁
Temperature (K)	200	200	200
a, b, c (Å)	24.3426 (18), 10.4266 (7), 7.8315 (6)	24.4783 (19), 10.4577 (9), 8.0978 (7)	24.650 (3), 10.4373 (9), 8.3992 (7)
V (Å³)	1987.7 (3)	2072.9 (3)	2160.9 (4)
Z	4	4	4
Radiation type	Mo Kα	Mo Kα	Mo Kα
μ (mm⁻¹)	3.83	7.94	6.46
Crystal size (mm)	0.35 × 0.22 × 0.11	0.35 × 0.20 × 0.12	0.40 × 0.22 × 0.10

Data collection
Diffractometer	Oxford Diffraction Gemini-S CCD-detector	Oxford Diffraction Gemini-S CCD-detector	Oxford Diffraction Gemini-S CCD-detector
Absorption correction	Multi-scan (CrysAlis PRO; Rigaku OD, 2015 $[Rigaku OD (2015). CrysAlis PRO. Rigaku Oxford Diffraction Ltd., Yarnton, England.]$ )	Multi-scan (CrysAlis PRO; Rigaku OD, 2015 $[Rigaku OD (2015). CrysAlis PRO. Rigaku Oxford Diffraction Ltd., Yarnton, England.]$ )	Multi-scan (CrysAlis PRO; Rigaku OD, 2015 $[Rigaku OD (2015). CrysAlis PRO. Rigaku Oxford Diffraction Ltd., Yarnton, England.]$ )
T_min, T_max	0.650, 0.980	0.375, 0.980	0.217, 0.980
No. of measured, independent and observed [I > 2σ(I)] reflections	2874, 1834, 1710	3623, 2093, 1899	4941, 1883, 1787
R_int	0.020	0.026	0.030
(sin θ/λ)_max (Å⁻¹)	0.688	0.683	0.687

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.030, 0.125, 1.23	0.032, 0.072, 1.03	0.041, 0.160, 1.18
No. of reflections	1834	2093	1883
No. of parameters	145	146	145
No. of restraints	8	8	8
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement	H atoms treated by a mixture of independent and constrained refinement	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.50, −0.84	0.70, −0.46	1.69, −1.00
Absolute structure	Flack (1983 ), 1281 Friedel pairs	Flack (1983), 1309 Friedel pairs	Flack (1983), 1405 Friedel pairs
Absolute structure parameter	0.03 (2)	−0.008 (12)	0.10 (4)
Computer programs: CrysAlis PRO (Rigaku OD, 2015 $[Rigaku OD (2015). CrysAlis PRO. Rigaku Oxford Diffraction Ltd., Yarnton, England.]$ ), SIR92 (Altomare et al., 1993 ), SHELXL97 (Sheldrick, 2008 ) within WinGX (Farrugia, 2012 ) and PLATON (Spek, 2009 ).

Supporting information

CCDC references: 1526425; 1526424; 1526423

Crystal structure: contains datablocks global, I, II, III. DOI: https://doi.org/10.1107/S2056989017000445/wm5350sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989017000445/wm5350Isup2.hkl

Structure factors: contains datablock II. DOI: https://doi.org/10.1107/S2056989017000445/wm5350IIsup3.hkl

Structure factors: contains datablock III. DOI: https://doi.org/10.1107/S2056989017000445/wm5350IIIsup4.hkl

checkCIF report

Computing details top

For all compounds, data collection: CrysAlis PRO (Rigaku OD, 2015); cell refinement: CrysAlis PRO (Rigaku OD, 2015); data reduction: CrysAlis PRO (Rigaku OD, 2015); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) within WinGX (Farrugia, 2012); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: PLATON (Spek, 2009).

(I) Poly[di-µ₃-4-aminophenylarsonato-tri-µ₂-aqua-dipotassium] top

Crystal data top

[K₂(C₆H₇AsNO₃)₂(H₂O)₃]	F(000) = 1128
M_r = 564.34	D_x = 1.886 Mg m⁻³
Orthorhombic, Cmc2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c -2	Cell parameters from 1421 reflections
a = 24.3426 (18) Å	θ = 4.1–28.7°
b = 10.4266 (7) Å	µ = 3.83 mm⁻¹
c = 7.8315 (6) Å	T = 200 K
V = 1987.7 (3) Å³	Prism, colourless
Z = 4	0.35 × 0.22 × 0.11 mm

Data collection top

Oxford Diffraction Gemini-S CCD-detector diffractometer	1834 independent reflections
Radiation source: Enhance (Mo) X-ray source	1710 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.020
Detector resolution: 16.077 pixels mm^-1	θ_max = 29.3°, θ_min = 3.2°
ω scans	h = −32→17
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2015)	k = −13→13
T_min = 0.650, T_max = 0.980	l = −9→10
2874 measured reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.030	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.125	w = 1/[σ²(F_o²) + (0.0744P)²] where P = (F_o² + 2F_c²)/3
S = 1.23	(Δ/σ)_max = 0.001
1834 reflections	Δρ_max = 0.50 e Å⁻³
145 parameters	Δρ_min = −0.84 e Å⁻³
8 restraints	Absolute structure: Flack (1983), 1281 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.03 (2)

Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles

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 > 2sigma(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 (Å²) top

	x	y	z	U_iso*/U_eq
As1	0.60155 (2)	0.63813 (4)	0.55509 (10)	0.0164 (2)
K1	0.50000	0.94523 (15)	0.5457 (3)	0.0224 (4)
K2	0.50000	0.63621 (19)	0.2140 (3)	0.0279 (6)
O1W	0.5845 (2)	1.0465 (4)	0.7396 (6)	0.0260 (12)
O2W	0.50000	0.7951 (6)	−0.1067 (9)	0.0263 (19)
O11	0.57103 (16)	0.7477 (4)	0.4358 (6)	0.0227 (12)
O12	0.5720 (2)	0.4898 (4)	0.5138 (6)	0.0333 (16)
O13	0.59063 (19)	0.6581 (4)	0.7630 (7)	0.0247 (14)
N4	0.8483 (2)	0.6311 (5)	0.4372 (8)	0.0243 (17)
C1	0.6778 (3)	0.6280 (5)	0.5052 (8)	0.0197 (16)
C2	0.7027 (3)	0.7225 (5)	0.4072 (8)	0.0203 (16)
C3	0.7583 (3)	0.7230 (5)	0.3828 (8)	0.0230 (17)
C4	0.7918 (3)	0.6313 (5)	0.4615 (7)	0.0170 (17)
C5	0.7669 (2)	0.5344 (4)	0.5574 (10)	0.0203 (14)
C6	0.7104 (2)	0.5332 (5)	0.5803 (8)	0.0197 (16)
H2	0.68080	0.78760	0.35650	0.0240*
H3	0.77440	0.78640	0.31150	0.0270*
H5	0.78880	0.46900	0.60720	0.0240*
H6	0.69380	0.46780	0.64730	0.0240*
H11W	0.608 (2)	0.998 (6)	0.795 (9)	0.0300*
H12	0.585 (3)	0.450 (6)	0.425 (6)	0.0300*
H12W	0.582 (3)	1.116 (4)	0.806 (8)	0.0300*
H21W	0.525 (2)	0.781 (7)	−0.181 (7)	0.0300*
H41	0.866 (3)	0.622 (5)	0.532 (5)	0.0240*
H42	0.863 (3)	0.683 (6)	0.363 (7)	0.0240*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
As1	0.0178 (3)	0.0148 (3)	0.0167 (3)	−0.0020 (2)	0.0030 (3)	−0.0007 (3)
K1	0.0198 (7)	0.0217 (7)	0.0256 (8)	0.0000	0.0000	−0.0055 (9)
K2	0.0186 (9)	0.0387 (11)	0.0264 (10)	0.0000	0.0000	−0.0114 (8)
O1W	0.028 (2)	0.023 (2)	0.027 (2)	0.0021 (19)	−0.006 (2)	−0.001 (2)
O2W	0.018 (3)	0.027 (3)	0.034 (4)	0.0000	0.0000	−0.003 (3)
O11	0.019 (2)	0.026 (2)	0.023 (2)	−0.0026 (17)	0.0023 (18)	0.0053 (18)
O12	0.037 (3)	0.022 (2)	0.041 (3)	−0.0120 (19)	0.022 (2)	−0.014 (2)
O13	0.023 (2)	0.024 (2)	0.027 (3)	0.0033 (19)	0.008 (2)	0.004 (2)
N4	0.019 (3)	0.024 (3)	0.030 (3)	0.002 (2)	−0.001 (2)	0.002 (2)
C1	0.022 (3)	0.015 (2)	0.022 (3)	−0.001 (2)	0.001 (2)	−0.002 (2)
C2	0.022 (3)	0.017 (2)	0.022 (3)	0.007 (2)	−0.001 (2)	0.000 (2)
C3	0.026 (3)	0.018 (3)	0.025 (3)	−0.003 (2)	0.006 (2)	0.011 (3)
C4	0.025 (3)	0.021 (3)	0.005 (3)	0.005 (2)	0.005 (2)	−0.0027 (19)
C5	0.025 (2)	0.013 (2)	0.023 (3)	0.0061 (18)	−0.002 (3)	0.003 (3)
C6	0.024 (3)	0.016 (2)	0.019 (3)	0.0002 (19)	0.007 (2)	0.001 (2)

Geometric parameters (Å, º) top

K1—O1W	2.766 (5)	O2W—H21W	0.86 (5)
K1—O11	2.824 (4)	O2W—H21Wⁱⁱ	0.86 (5)
K1—O2Wⁱ	2.959 (7)	O12—H12	0.87 (6)
K1—O1Wⁱⁱ	2.766 (5)	N4—C4	1.389 (9)
K1—O11ⁱⁱ	2.824 (4)	N4—H41	0.86 (5)
K2—O2W	3.009 (7)	N4—H42	0.87 (6)
K2—O11	2.713 (5)	C1—C2	1.388 (8)
K2—O12ⁱⁱⁱ	2.694 (5)	C1—C6	1.397 (8)
K2—O11ⁱⁱ	2.713 (5)	C2—C3	1.367 (10)
K2—O12^iv	2.694 (5)	C3—C4	1.400 (9)
As1—O11	1.652 (4)	C4—C5	1.397 (8)
As1—O12	1.736 (4)	C5—C6	1.387 (7)
As1—O13	1.663 (5)	C2—H2	0.9500
As1—C1	1.900 (7)	C3—H3	0.9500
O1W—H11W	0.88 (6)	C5—H5	0.9500
O1W—H12W	0.89 (5)	C6—H6	0.9500

O11—As1—O12	108.9 (2)	K1—O1W—H12W	125 (5)
O11—As1—O13	113.3 (2)	H11W—O1W—H12W	103 (6)
O11—As1—C1	111.2 (2)	K1^v—O2W—H21W	116 (5)
O12—As1—O13	103.2 (2)	H21W—O2W—H21Wⁱⁱ	91 (5)
O12—As1—C1	108.5 (2)	K1^v—O2W—H21Wⁱⁱ	116 (5)
O13—As1—C1	111.4 (3)	K2—O2W—H21W	118 (4)
O1W—K1—O11	89.45 (13)	K2—O2W—H21Wⁱⁱ	118 (4)
O1W—K1—O2Wⁱ	82.66 (13)	K2^vi—O12—H12	118 (4)
O1W—K1—O1Wⁱⁱ	96.08 (15)	As1—O12—H12	115 (4)
O1W—K1—O11ⁱⁱ	154.31 (14)	C4—N4—H41	112 (4)
O2Wⁱ—K1—O11	122.99 (14)	H41—N4—H42	116 (6)
O1Wⁱⁱ—K1—O11	154.31 (14)	C4—N4—H42	120 (5)
O11—K1—O11ⁱⁱ	75.52 (12)	As1—C1—C6	120.5 (4)
O1Wⁱⁱ—K1—O2Wⁱ	82.66 (13)	As1—C1—C2	120.1 (5)
O2Wⁱ—K1—O11ⁱⁱ	122.99 (14)	C2—C1—C6	119.1 (6)
O1Wⁱⁱ—K1—O11ⁱⁱ	89.45 (13)	C1—C2—C3	120.8 (6)
O2W—K2—O11	107.37 (14)	C2—C3—C4	120.9 (6)
O2W—K2—O12ⁱⁱⁱ	77.45 (14)	C3—C4—C5	118.6 (6)
O2W—K2—O11ⁱⁱ	107.37 (14)	N4—C4—C3	121.2 (5)
O2W—K2—O12^iv	77.45 (14)	N4—C4—C5	120.2 (5)
O11—K2—O12ⁱⁱⁱ	175.18 (16)	C4—C5—C6	120.4 (5)
O11—K2—O11ⁱⁱ	79.20 (14)	C1—C6—C5	120.2 (5)
O11—K2—O12^iv	99.61 (13)	C1—C2—H2	120.00
O11ⁱⁱ—K2—O12ⁱⁱⁱ	99.61 (13)	C3—C2—H2	120.00
O12ⁱⁱⁱ—K2—O12^iv	81.18 (15)	C2—C3—H3	120.00
O11ⁱⁱ—K2—O12^iv	175.18 (16)	C4—C3—H3	120.00
K1^v—O2W—K2	99.6 (2)	C4—C5—H5	120.00
K1—O11—K2	96.75 (13)	C6—C5—H5	120.00
As1—O12—K2^vi	126.6 (2)	C1—C6—H6	120.00
K1—O1W—H11W	122 (4)	C5—C6—H6	120.00

O12—As1—O11—K1	109.9 (3)	O11ⁱⁱ—K1—O11—K2	25.38 (14)
O12—As1—O11—K2	−6.6 (3)	O1W—K1—O11ⁱⁱ—K2	−81.4 (4)
O13—As1—O11—K1	−4.3 (3)	O11—K1—O11ⁱⁱ—K2	−25.38 (14)
O13—As1—O11—K2	−120.8 (2)	O2W—K2—O11—As1	−146.8 (2)
C1—As1—O11—K1	−130.6 (3)	O2W—K2—O11—K1	78.91 (15)
C1—As1—O11—K2	112.9 (2)	O11ⁱⁱ—K2—O11—As1	108.2 (2)
O11—As1—O12—K2^vi	−103.8 (3)	O11ⁱⁱ—K2—O11—K1	−26.09 (14)
O13—As1—O12—K2^vi	16.9 (3)	O12^iv—K2—O11—As1	−67.1 (2)
C1—As1—O12—K2^vi	135.1 (3)	O12^iv—K2—O11—K1	158.66 (14)
O11—As1—C1—C2	12.4 (6)	O11—K2—O11ⁱⁱ—K1	26.09 (14)
O11—As1—C1—C6	−174.0 (5)	As1—C1—C2—C3	174.1 (5)
O12—As1—C1—C2	132.2 (5)	C6—C1—C2—C3	0.5 (9)
O12—As1—C1—C6	−54.3 (5)	As1—C1—C6—C5	−173.3 (5)
O13—As1—C1—C2	−114.9 (5)	C2—C1—C6—C5	0.3 (9)
O13—As1—C1—C6	58.6 (5)	C1—C2—C3—C4	−2.6 (9)
O1W—K1—O11—As1	61.8 (3)	C2—C3—C4—N4	179.9 (6)
O1W—K1—O11—K2	−175.68 (15)	C2—C3—C4—C5	3.8 (9)
O2Wⁱ—K1—O11—As1	142.7 (2)	N4—C4—C5—C6	−179.2 (6)
O1Wⁱⁱ—K1—O11—As1	−41.1 (5)	C3—C4—C5—C6	−3.0 (9)
O1Wⁱⁱ—K1—O11—K2	81.4 (4)	C4—C5—C6—C1	1.0 (9)
O11ⁱⁱ—K1—O11—As1	−97.1 (3)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H11W···N4^vii	0.88 (6)	2.05 (6)	2.915 (7)	171 (5)
O1W—H12W···O11^viii	0.89 (5)	1.77 (5)	2.660 (6)	175 (7)
O2W—H21W···O13^ix	0.86 (5)	2.09 (6)	2.819 (6)	142 (6)
O12—H12···O13^iv	0.87 (6)	1.70 (6)	2.538 (7)	160 (7)
N4—H41···O1W^x	0.86 (5)	2.17 (5)	3.010 (7)	164 (5)
N4—H42···O13^xi	0.87 (6)	2.15 (6)	2.984 (7)	160 (5)

Symmetry codes: (iv) x, −y+1, z−1/2; (vii) −x+3/2, −y+3/2, z+1/2; (viii) x, −y+2, z+1/2; (ix) x, y, z−1; (x) −x+3/2, y−1/2, z; (xi) −x+3/2, −y+3/2, z−1/2.

(II) Poly[di-µ₃-4-aminophenylarsonato-tri-µ₂-aqua-dirubidium] top

Crystal data top

[Rb₂(C₆H₇AsNO₃)₂(H₂O)₃]	F(000) = 1272
M_r = 657.08	D_x = 2.105 Mg m⁻³
Orthorhombic, Cmc2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c -2	Cell parameters from 1374 reflections
a = 24.4783 (19) Å	θ = 4.0–28.7°
b = 10.4577 (9) Å	µ = 7.94 mm⁻¹
c = 8.0978 (7) Å	T = 200 K
V = 2072.9 (3) Å³	Prism, colourless
Z = 4	0.35 × 0.20 × 0.12 mm

Data collection top

Oxford Diffraction Gemini-S CCD-detector diffractometer	2093 independent reflections
Radiation source: Enhance (Mo) X-ray source	1899 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.026
Detector resolution: 16.077 pixels mm^-1	θ_max = 29.0°, θ_min = 3.9°
ω scans	h = −33→15
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2015)	k = −14→13
T_min = 0.375, T_max = 0.980	l = −10→10
3623 measured reflections

Refinement top

Refinement on F²	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F² > 2σ(F²)] = 0.032	w = 1/[σ²(F_o²) + (0.0392P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.072	(Δ/σ)_max = 0.003
S = 1.03	Δρ_max = 0.70 e Å⁻³
2093 reflections	Δρ_min = −0.46 e Å⁻³
146 parameters	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
8 restraints	Extinction coefficient: 0.00306 (19)
Primary atom site location: structure-invariant direct methods	Absolute structure: Flack (1983), 1309 Friedel pairs
Secondary atom site location: difference Fourier map	Absolute structure parameter: −0.008 (12)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Rb1	0.50000	0.94747 (5)	0.57916 (11)	0.0264 (2)
Rb2	0.50000	0.63207 (8)	0.24818 (10)	0.0376 (3)
As1	0.60556 (2)	0.63552 (4)	0.58879 (6)	0.0200 (1)
O1W	0.58793 (16)	1.0545 (3)	0.7791 (5)	0.0333 (11)
O2W	0.50000	0.7864 (5)	−0.0920 (7)	0.0337 (17)
O11	0.57535 (14)	0.7458 (3)	0.4753 (4)	0.0302 (11)
O12	0.57765 (17)	0.4882 (3)	0.5436 (5)	0.0404 (13)
O13	0.59344 (15)	0.6516 (3)	0.7898 (4)	0.0275 (11)
N4	0.85111 (17)	0.6329 (4)	0.4734 (6)	0.0287 (16)
C1	0.68166 (19)	0.6279 (4)	0.5443 (6)	0.0200 (14)
C2	0.7060 (2)	0.7197 (5)	0.4430 (6)	0.0250 (16)
C3	0.7614 (2)	0.7222 (5)	0.4197 (7)	0.0270 (17)
C4	0.7946 (2)	0.6315 (4)	0.4982 (6)	0.0230 (16)
C5	0.77044 (19)	0.5380 (4)	0.5957 (8)	0.0270 (14)
C6	0.7146 (2)	0.5357 (4)	0.6178 (6)	0.0260 (16)
H2	0.68380	0.78150	0.38940	0.0300*
H3	0.77730	0.78530	0.35030	0.0320*
H5	0.79260	0.47510	0.64760	0.0320*
H6	0.69850	0.47060	0.68370	0.0310*
H11W	0.6067 (19)	1.001 (4)	0.842 (6)	0.0370*
H12	0.582 (2)	0.459 (5)	0.445 (3)	0.0370*
H12W	0.589 (3)	1.127 (3)	0.833 (6)	0.0370*
H21W	0.5290 (15)	0.741 (4)	−0.120 (7)	0.0370*
H41	0.864 (2)	0.689 (4)	0.407 (6)	0.0300*
H42	0.8680 (19)	0.613 (4)	0.566 (4)	0.0300*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Rb1	0.0241 (3)	0.0282 (3)	0.0268 (3)	0.0000	0.0000	−0.0051 (4)
Rb2	0.0227 (4)	0.0597 (5)	0.0304 (4)	0.0000	0.0000	−0.0179 (4)
As1	0.0210 (2)	0.0183 (2)	0.0206 (2)	−0.0019 (2)	0.0036 (2)	−0.0007 (3)
O1W	0.032 (2)	0.0309 (19)	0.037 (2)	−0.0008 (16)	−0.0036 (19)	−0.0005 (18)
O2W	0.032 (3)	0.027 (3)	0.042 (3)	0.0000	0.0000	−0.006 (2)
O11	0.0206 (19)	0.037 (2)	0.033 (2)	−0.0005 (16)	−0.0041 (16)	0.0069 (16)
O12	0.046 (2)	0.0303 (18)	0.045 (3)	−0.0176 (17)	0.0261 (19)	−0.0182 (19)
O13	0.036 (2)	0.0257 (18)	0.0207 (18)	0.0053 (15)	0.0064 (16)	0.0031 (15)
N4	0.019 (2)	0.035 (3)	0.032 (3)	0.0024 (18)	0.0042 (19)	0.006 (2)
C1	0.019 (2)	0.021 (2)	0.020 (3)	0.0003 (17)	0.0009 (18)	−0.0017 (18)
C2	0.025 (3)	0.021 (2)	0.029 (3)	0.001 (2)	0.002 (2)	0.005 (2)
C3	0.023 (3)	0.025 (3)	0.033 (3)	0.001 (2)	0.006 (2)	0.009 (2)
C4	0.025 (3)	0.021 (2)	0.023 (3)	0.0018 (19)	0.004 (2)	−0.0043 (19)
C5	0.031 (2)	0.020 (2)	0.030 (3)	0.0078 (17)	0.003 (3)	0.003 (3)
C6	0.036 (3)	0.018 (2)	0.024 (3)	−0.0023 (19)	0.006 (2)	0.0040 (19)

Geometric parameters (Å, º) top

Rb1—O1W	2.917 (4)	O1W—H12W	0.88 (4)
Rb1—O11	2.925 (3)	O2W—H21W	0.88 (4)
Rb1—O2Wⁱ	3.151 (6)	O2W—H21W^iv	0.88 (4)
Rb1—O1Wⁱⁱ	3.246 (4)	O12—H12	0.86 (3)
Rb1—O2Wⁱⁱⁱ	3.109 (5)	N4—C4	1.398 (6)
Rb1—O1W^iv	2.917 (4)	N4—H41	0.86 (5)
Rb1—O11^iv	2.925 (3)	N4—H42	0.88 (4)
Rb1—O1W^v	3.246 (4)	C1—C2	1.396 (7)
Rb2—O2W	3.193 (6)	C1—C6	1.391 (6)
Rb2—O11	2.863 (3)	C2—C3	1.369 (7)
Rb2—O12^vi	2.818 (4)	C3—C4	1.402 (7)
Rb2—O11^iv	2.863 (3)	C4—C5	1.389 (7)
Rb2—O12^vii	2.818 (4)	C5—C6	1.379 (7)
As1—O11	1.650 (3)	C2—H2	0.9500
As1—O12	1.725 (3)	C3—H3	0.9500
As1—O13	1.663 (3)	C5—H5	0.9500
As1—C1	1.899 (5)	C6—H6	0.9500
O1W—H11W	0.89 (5)

O1W—Rb1—O11	88.34 (10)	Rb1—O1W—Rb1ⁱⁱⁱ	85.63 (10)
O1W—Rb1—O2Wⁱ	74.69 (10)	Rb1^viii—O2W—Rb2	178.05 (19)
O1W—Rb1—O1Wⁱⁱ	155.13 (9)	Rb1ⁱⁱ—O2W—Rb2	93.89 (15)
O1W—Rb1—O2Wⁱⁱⁱ	84.49 (10)	Rb1^viii—O2W—Rb1ⁱⁱ	84.16 (13)
O1W—Rb1—O1W^iv	95.12 (11)	Rb1—O11—Rb2	94.47 (10)
O1W—Rb1—O11^iv	154.37 (10)	Rb1—O11—As1	128.79 (16)
O1W—Rb1—O1W^v	85.91 (10)	Rb2—O11—As1	110.86 (15)
O2Wⁱ—Rb1—O11	81.81 (10)	Rb2^ix—O12—As1	122.77 (19)
O1Wⁱⁱ—Rb1—O11	101.44 (9)	Rb1ⁱⁱⁱ—O1W—H12W	70 (4)
O2Wⁱⁱⁱ—Rb1—O11	121.14 (10)	Rb1—O1W—H12W	129 (5)
O1W^iv—Rb1—O11	154.37 (10)	H11W—O1W—H12W	104 (5)
O11—Rb1—O11^iv	78.18 (9)	Rb1—O1W—H11W	117 (3)
O1W^v—Rb1—O11	50.37 (9)	Rb1ⁱⁱⁱ—O1W—H11W	85 (3)
O1Wⁱⁱ—Rb1—O2Wⁱ	128.99 (8)	Rb2—O2W—H21W^iv	87 (4)
O2Wⁱ—Rb1—O2Wⁱⁱⁱ	148.79 (14)	Rb1^viii—O2W—H21W	94 (4)
O1W^iv—Rb1—O2Wⁱ	74.69 (10)	Rb2—O2W—H21W	87 (4)
O2Wⁱ—Rb1—O11^iv	81.81 (10)	H21W—O2W—H21W^iv	107 (4)
O1W^v—Rb1—O2Wⁱ	128.99 (8)	Rb1^viii—O2W—H21W^iv	94 (4)
O1Wⁱⁱ—Rb1—O2Wⁱⁱⁱ	70.85 (9)	Rb1ⁱⁱ—O2W—H21W	127 (3)
O1Wⁱⁱ—Rb1—O1W^iv	85.91 (10)	Rb1ⁱⁱ—O2W—H21W^iv	127 (3)
O1Wⁱⁱ—Rb1—O11^iv	50.37 (9)	Rb2^ix—O12—H12	118 (3)
O1Wⁱⁱ—Rb1—O1W^v	83.07 (10)	As1—O12—H12	118 (3)
O1W^iv—Rb1—O2Wⁱⁱⁱ	84.49 (10)	C4—N4—H41	118 (3)
O2Wⁱⁱⁱ—Rb1—O11^iv	121.14 (10)	C4—N4—H42	110 (3)
O1W^v—Rb1—O2Wⁱⁱⁱ	70.85 (9)	H41—N4—H42	122 (4)
O1W^iv—Rb1—O11^iv	88.34 (10)	C2—C1—C6	118.7 (4)
O1W^iv—Rb1—O1W^v	155.13 (9)	As1—C1—C2	120.1 (3)
O1W^v—Rb1—O11^iv	101.44 (9)	As1—C1—C6	121.1 (3)
O2W—Rb2—O11	110.13 (10)	C1—C2—C3	121.1 (5)
O2W—Rb2—O12^vi	73.64 (10)	C2—C3—C4	119.9 (5)
O2W—Rb2—O11^iv	110.13 (10)	N4—C4—C5	120.7 (4)
O2W—Rb2—O12^vii	73.64 (10)	N4—C4—C3	120.1 (4)
O11—Rb2—O12^vi	176.01 (11)	C3—C4—C5	119.2 (4)
O11—Rb2—O11^iv	80.20 (10)	C4—C5—C6	120.5 (4)
O11—Rb2—O12^vii	97.38 (11)	C1—C6—C5	120.5 (4)
O11^iv—Rb2—O12^vi	97.38 (11)	C1—C2—H2	119.00
O12^vi—Rb2—O12^vii	84.84 (12)	C3—C2—H2	119.00
O11^iv—Rb2—O12^vii	176.01 (11)	C2—C3—H3	120.00
O11—As1—O12	109.20 (17)	C4—C3—H3	120.00
O11—As1—O13	113.24 (16)	C4—C5—H5	120.00
O11—As1—C1	111.30 (18)	C6—C5—H5	120.00
O12—As1—O13	103.14 (18)	C1—C6—H6	120.00
O12—As1—C1	108.11 (19)	C5—C6—H6	120.00
O13—As1—C1	111.40 (19)

O11—Rb1—O1W—Rb1ⁱⁱⁱ	−128.95 (9)	O13—As1—O11—Rb1	−4.5 (3)
O1W—Rb1—O11—Rb2	−175.57 (10)	O13—As1—O11—Rb2	−118.92 (17)
O1W—Rb1—O11—As1	63.0 (2)	C1—As1—O11—Rb1	−130.9 (2)
O2Wⁱ—Rb1—O11—As1	−11.8 (2)	C1—As1—O11—Rb2	114.66 (18)
O1Wⁱⁱ—Rb1—O11—Rb2	−18.62 (11)	O11—As1—O12—Rb2^ix	−101.6 (2)
O1Wⁱⁱ—Rb1—O11—As1	−140.0 (2)	O13—As1—O12—Rb2^ix	19.1 (2)
O2Wⁱⁱⁱ—Rb1—O11—As1	145.56 (19)	C1—As1—O12—Rb2^ix	137.2 (2)
O1W^iv—Rb1—O11—Rb2	86.1 (2)	O11—As1—C1—C2	7.8 (4)
O1W^iv—Rb1—O11—As1	−35.4 (4)	O11—As1—C1—C6	−175.6 (4)
O11^iv—Rb1—O11—Rb2	26.37 (9)	O12—As1—C1—C2	127.7 (4)
O11^iv—Rb1—O11—As1	−95.1 (2)	O12—As1—C1—C6	−55.6 (4)
O1W^v—Rb1—O11—Rb2	−89.51 (13)	O13—As1—C1—C2	−119.7 (4)
O1W^v—Rb1—O11—As1	149.1 (3)	O13—As1—C1—C6	57.0 (4)
O1W—Rb1—O11^iv—Rb2	−86.1 (2)	As1—C1—C2—C3	174.8 (4)
O11—Rb1—O11^iv—Rb2	−26.37 (9)	C6—C1—C2—C3	−2.0 (7)
O2W—Rb2—O11—Rb1	81.20 (11)	As1—C1—C6—C5	−174.4 (4)
O2W—Rb2—O11—As1	−144.19 (15)	C2—C1—C6—C5	2.4 (7)
O11^iv—Rb2—O11—Rb1	−26.79 (9)	C1—C2—C3—C4	0.0 (8)
O11^iv—Rb2—O11—As1	107.83 (17)	C2—C3—C4—N4	179.3 (5)
O12^vii—Rb2—O11—Rb1	156.43 (10)	C2—C3—C4—C5	1.6 (8)
O12^vii—Rb2—O11—As1	−68.96 (17)	N4—C4—C5—C6	−179.0 (5)
O11—Rb2—O11^iv—Rb1	26.79 (9)	C3—C4—C5—C6	−1.3 (8)
O12—As1—O11—Rb1	109.8 (2)	C4—C5—C6—C1	−0.8 (8)
O12—As1—O11—Rb2	−4.6 (2)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H11W···N4^x	0.89 (5)	2.04 (4)	2.923 (6)	176 (5)
O2W—H21W···O13^viii	0.88 (4)	1.97 (4)	2.852 (5)	173 (5)
O12—H12···O13^vii	0.86 (3)	1.73 (4)	2.552 (5)	158 (5)
N4—H41···O13^xi	0.86 (5)	2.18 (4)	3.022 (5)	167 (4)
N4—H42···O1W^xii	0.88 (4)	2.13 (4)	3.005 (6)	176 (4)

Symmetry codes: (vii) x, −y+1, z−1/2; (viii) x, y, z−1; (x) −x+3/2, −y+3/2, z+1/2; (xi) −x+3/2, −y+3/2, z−1/2; (xii) −x+3/2, y−1/2, z.

(III) Poly[di-µ₃-4-aminophenylarsonato-tri-µ₂-aqua-dicaesium] top

Crystal data top

[Cs₂(C₆H₇AsNO₃)₂(H₂O)₃]	F(000) = 1416
M_r = 751.96	D_x = 2.311 Mg m⁻³
Orthorhombic, Cmc2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c -2	Cell parameters from 1999 reflections
a = 24.650 (3) Å	θ = 4.0–28.9°
b = 10.4373 (9) Å	µ = 6.46 mm⁻¹
c = 8.3992 (7) Å	T = 200 K
V = 2160.9 (4) Å³	Prism, colourless
Z = 4	0.40 × 0.22 × 0.10 mm

Data collection top

Oxford Diffraction Gemini-S CCD-detector diffractometer	1883 independent reflections
Radiation source: Enhance Mo X-ray source	1787 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.030
Detector resolution: 16.077 pixels mm^-1	θ_max = 29.3°, θ_min = 3.2°
ω scans	h = −33→29
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2015)	k = −14→13
T_min = 0.217, T_max = 0.980	l = −11→6
4941 measured reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.041	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.160	w = 1/[σ²(F_o²) + (0.1178P)²] where P = (F_o² + 2F_c²)/3
S = 1.18	(Δ/σ)_max = 0.001
1883 reflections	Δρ_max = 1.69 e Å⁻³
145 parameters	Δρ_min = −1.00 e Å⁻³
8 restraints	Absolute structure: Flack (1983), 1405 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.10 (4)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Cs1	0.50000	0.95299 (7)	0.67229 (13)	0.0217 (2)
Cs2	0.50000	0.62982 (10)	0.99928 (13)	0.0311 (3)
As1	0.61041 (4)	0.63299 (7)	0.65867 (12)	0.0166 (3)
O1W	0.5936 (4)	1.0619 (7)	0.4690 (11)	0.026 (3)
O2W	0.50000	0.7680 (11)	0.3558 (16)	0.027 (3)
O11	0.5799 (3)	0.7443 (8)	0.7661 (11)	0.028 (3)
O12	0.5841 (4)	0.4827 (8)	0.7086 (11)	0.036 (3)
O13	0.5962 (3)	0.6457 (7)	0.4668 (11)	0.024 (2)
N4	0.8542 (4)	0.6351 (9)	0.7686 (14)	0.025 (3)
C1	0.6861 (5)	0.6283 (7)	0.6996 (13)	0.016 (3)
C2	0.7088 (5)	0.7189 (9)	0.7999 (14)	0.022 (3)
C3	0.7634 (5)	0.7201 (9)	0.8256 (18)	0.025 (3)
C4	0.7983 (5)	0.6344 (9)	0.7490 (14)	0.022 (3)
C5	0.7752 (5)	0.5399 (9)	0.6487 (19)	0.031 (4)
C6	0.7202 (5)	0.5380 (8)	0.6236 (15)	0.023 (3)
H2	0.68620	0.78020	0.85100	0.0260*
H3	0.77820	0.78100	0.89760	0.0300*
H5	0.79770	0.47800	0.59880	0.0370*
H6	0.70480	0.47550	0.55480	0.0270*
H11W	0.624 (3)	1.039 (12)	0.420 (15)	0.0340*
H12	0.578 (7)	0.493 (15)	0.811 (5)	0.0340*
H12W	0.589 (4)	1.126 (12)	0.400 (12)	0.0340*
H21W	0.529 (4)	0.773 (13)	0.418 (16)	0.0340*
H41	0.865 (6)	0.602 (12)	0.685 (18)	0.0270*
H42	0.870 (6)	0.706 (11)	0.81 (2)	0.0270*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cs1	0.0185 (4)	0.0261 (4)	0.0204 (4)	0.0000	0.0000	0.0024 (4)
Cs2	0.0174 (5)	0.0525 (6)	0.0233 (5)	0.0000	0.0000	0.0136 (5)
As1	0.0146 (5)	0.0182 (4)	0.0169 (5)	−0.0016 (3)	−0.0029 (5)	0.0004 (4)
O1W	0.017 (4)	0.035 (4)	0.026 (5)	0.000 (3)	0.009 (4)	0.002 (4)
O2W	0.020 (6)	0.031 (5)	0.030 (7)	0.0000	0.0000	0.002 (5)
O11	0.020 (4)	0.032 (4)	0.031 (5)	−0.002 (3)	0.007 (4)	−0.005 (3)
O12	0.042 (5)	0.033 (4)	0.032 (5)	−0.021 (4)	−0.024 (4)	0.007 (4)
O13	0.019 (4)	0.029 (4)	0.025 (4)	0.005 (3)	0.000 (4)	0.001 (3)
N4	0.020 (5)	0.026 (4)	0.030 (5)	0.003 (3)	−0.015 (5)	−0.004 (4)
C1	0.019 (5)	0.015 (4)	0.014 (4)	0.000 (3)	−0.004 (4)	0.001 (3)
C2	0.027 (6)	0.020 (4)	0.019 (5)	0.006 (4)	−0.009 (4)	−0.011 (4)
C3	0.022 (5)	0.024 (4)	0.030 (6)	0.003 (4)	0.006 (6)	−0.002 (5)
C4	0.021 (6)	0.021 (4)	0.023 (6)	0.004 (4)	0.002 (5)	0.006 (4)
C5	0.028 (6)	0.024 (4)	0.041 (8)	0.006 (4)	−0.005 (6)	−0.013 (5)
C6	0.020 (5)	0.020 (4)	0.029 (6)	−0.003 (3)	−0.005 (5)	−0.002 (4)

Geometric parameters (Å, º) top

Cs1—O1W	3.087 (9)	O1W—H12W	0.89 (12)
Cs1—O2W	3.286 (13)	O2W—H21W	0.89 (12)
Cs1—O11	3.040 (8)	O2W—H21Wⁱⁱ	0.89 (12)
Cs1—O1Wⁱ	3.400 (10)	O12—H12	0.88 (5)
Cs1—O2Wⁱ	3.295 (12)	N4—C4	1.388 (16)
Cs1—O1Wⁱⁱ	3.087 (9)	N4—H41	0.83 (14)
Cs1—O11ⁱⁱ	3.040 (8)	N4—H42	0.91 (14)
Cs1—O1Wⁱⁱⁱ	3.400 (10)	C1—C2	1.385 (15)
Cs2—O11	3.024 (8)	C1—C6	1.415 (15)
Cs2—O2W^iv	3.324 (13)	C2—C3	1.363 (17)
Cs2—O12^v	2.961 (9)	C3—C4	1.398 (16)
Cs2—O11ⁱⁱ	3.024 (8)	C4—C5	1.417 (17)
Cs2—O12^vi	2.961 (9)	C5—C6	1.372 (18)
As1—O11	1.652 (9)	C2—H2	0.9500
As1—O12	1.748 (9)	C3—H3	0.9500
As1—O13	1.655 (9)	C5—H5	0.9500
As1—C1	1.898 (12)	C6—H6	0.9500
O1W—H11W	0.89 (9)

O1W—Cs1—O2W	76.6 (2)	Cs1—O1W—Cs1^vii	83.2 (2)
O1W—Cs1—O11	85.6 (2)	Cs1—O2W—Cs2^viii	169.7 (4)
O1W—Cs1—O1Wⁱ	158.4 (2)	Cs1—O2W—Cs1^vii	81.9 (3)
O1W—Cs1—O2Wⁱ	86.2 (2)	Cs1^vii—O2W—Cs2^viii	87.8 (3)
O1W—Cs1—O1Wⁱⁱ	96.7 (2)	Cs1—O11—Cs2	91.7 (2)
O1W—Cs1—O11ⁱⁱ	153.0 (2)	Cs1—O11—As1	131.1 (4)
O1W—Cs1—O1Wⁱⁱⁱ	85.1 (2)	Cs2—O11—As1	111.9 (4)
O2W—Cs1—O11	77.8 (2)	Cs2^ix—O12—As1	118.2 (4)
O1Wⁱ—Cs1—O2W	124.49 (19)	Cs1^vii—O1W—H12W	58 (7)
O2W—Cs1—O2Wⁱ	153.9 (3)	Cs1—O1W—H12W	123 (7)
O1Wⁱⁱ—Cs1—O2W	76.6 (2)	H11W—O1W—H12W	91 (11)
O2W—Cs1—O11ⁱⁱ	77.8 (2)	Cs1—O1W—H11W	142 (8)
O1Wⁱⁱⁱ—Cs1—O2W	124.49 (19)	Cs1^vii—O1W—H11W	103 (8)
O1Wⁱ—Cs1—O11	102.5 (2)	Cs1—O2W—H21Wⁱⁱ	59 (8)
O2Wⁱ—Cs1—O11	120.8 (2)	Cs2^viii—O2W—H21W	124 (7)
O1Wⁱⁱ—Cs1—O11	153.0 (2)	Cs1—O2W—H21W	59 (8)
O11—Cs1—O11ⁱⁱ	80.8 (2)	H21W—O2W—H21Wⁱⁱ	107 (11)
O1Wⁱⁱⁱ—Cs1—O11	48.5 (2)	Cs2^viii—O2W—H21Wⁱⁱ	124 (8)
O1Wⁱ—Cs1—O2Wⁱ	72.4 (2)	Cs1^vii—O2W—H21W	103 (8)
O1Wⁱ—Cs1—O1Wⁱⁱ	85.1 (2)	Cs1^vii—O2W—H21Wⁱⁱ	103 (9)
O1Wⁱ—Cs1—O11ⁱⁱ	48.5 (2)	Cs2^ix—O12—H12	121 (11)
O1Wⁱ—Cs1—O1Wⁱⁱⁱ	85.5 (2)	As1—O12—H12	101 (10)
O1Wⁱⁱ—Cs1—O2Wⁱ	86.2 (2)	C4—N4—H41	103 (10)
O2Wⁱ—Cs1—O11ⁱⁱ	120.8 (2)	C4—N4—H42	119 (8)
O1Wⁱⁱⁱ—Cs1—O2Wⁱ	72.4 (2)	H41—N4—H42	122 (13)
O1Wⁱⁱ—Cs1—O11ⁱⁱ	85.6 (2)	C2—C1—C6	119.3 (11)
O1Wⁱⁱ—Cs1—O1Wⁱⁱⁱ	158.4 (2)	As1—C1—C2	119.3 (8)
O1Wⁱⁱⁱ—Cs1—O11ⁱⁱ	102.5 (2)	As1—C1—C6	121.3 (8)
O2W^iv—Cs2—O11	114.3 (2)	C1—C2—C3	120.1 (11)
O11—Cs2—O12^v	175.8 (2)	C2—C3—C4	121.9 (11)
O11—Cs2—O11ⁱⁱ	81.3 (2)	N4—C4—C5	118.3 (10)
O11—Cs2—O12^vi	94.9 (2)	N4—C4—C3	123.6 (10)
O2W^iv—Cs2—O12^v	68.7 (2)	C3—C4—C5	118.2 (11)
O2W^iv—Cs2—O11ⁱⁱ	114.3 (2)	C4—C5—C6	119.9 (11)
O2W^iv—Cs2—O12^vi	68.7 (2)	C1—C6—C5	120.5 (10)
O11ⁱⁱ—Cs2—O12^v	94.9 (2)	C1—C2—H2	120.00
O12^v—Cs2—O12^vi	88.9 (3)	C3—C2—H2	120.00
O11ⁱⁱ—Cs2—O12^vi	175.8 (2)	C2—C3—H3	119.00
O11—As1—O12	109.3 (4)	C4—C3—H3	119.00
O11—As1—O13	112.3 (4)	C4—C5—H5	120.00
O11—As1—C1	111.5 (4)	C6—C5—H5	120.00
O12—As1—O13	103.1 (4)	C1—C6—H6	120.00
O12—As1—C1	107.3 (4)	C5—C6—H6	120.00
O13—As1—C1	112.8 (4)

O11—Cs1—O1W—Cs1^vii	126.4 (2)	O13—As1—O11—Cs1	3.5 (6)
O1W—Cs1—O11—Cs2	175.0 (2)	O13—As1—O11—Cs2	116.5 (4)
O1W—Cs1—O11—As1	−63.7 (5)	C1—As1—O11—Cs1	131.1 (5)
O2W—Cs1—O11—Cs2	−107.8 (2)	C1—As1—O11—Cs2	−115.8 (4)
O2W—Cs1—O11—As1	13.5 (5)	O11—As1—O12—Cs2^ix	98.9 (5)
O1Wⁱ—Cs1—O11—Cs2	15.3 (3)	O13—As1—O12—Cs2^ix	−20.8 (5)
O1Wⁱ—Cs1—O11—As1	136.6 (5)	C1—As1—O12—Cs2^ix	−140.0 (5)
O2Wⁱ—Cs1—O11—As1	−146.6 (5)	O11—As1—C1—C2	−4.7 (10)
O1Wⁱⁱ—Cs1—O11—Cs2	−88.9 (5)	O11—As1—C1—C6	178.4 (8)
O1Wⁱⁱ—Cs1—O11—As1	32.4 (9)	O12—As1—C1—C2	−124.4 (8)
O11ⁱⁱ—Cs1—O11—Cs2	−28.4 (2)	O12—As1—C1—C6	58.7 (9)
O11ⁱⁱ—Cs1—O11—As1	93.0 (5)	O13—As1—C1—C2	122.7 (8)
O1Wⁱⁱⁱ—Cs1—O11—Cs2	87.6 (3)	O13—As1—C1—C6	−54.2 (9)
O1Wⁱⁱⁱ—Cs1—O11—As1	−151.1 (6)	As1—C1—C2—C3	−177.4 (9)
O1W—Cs1—O11ⁱⁱ—Cs2	88.9 (5)	C6—C1—C2—C3	−0.5 (16)
O11—Cs1—O11ⁱⁱ—Cs2	28.4 (2)	As1—C1—C6—C5	176.9 (9)
O2W^iv—Cs2—O11—As1	139.6 (4)	C2—C1—C6—C5	0.0 (16)
O11ⁱⁱ—Cs2—O11—Cs1	28.5 (2)	C1—C2—C3—C4	2.2 (18)
O11ⁱⁱ—Cs2—O11—As1	−107.6 (4)	C2—C3—C4—N4	178.1 (11)
O12^vi—Cs2—O11—Cs1	−153.2 (2)	C2—C3—C4—C5	−3.4 (18)
O12^vi—Cs2—O11—As1	70.7 (4)	N4—C4—C5—C6	−178.5 (11)
O11—Cs2—O11ⁱⁱ—Cs1	−28.5 (2)	C3—C4—C5—C6	2.9 (18)
O12—As1—O11—Cs1	−110.3 (5)	C4—C5—C6—C1	−1.2 (18)
O12—As1—O11—Cs2	2.7 (5)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H11W···N4^x	0.89 (9)	2.28 (13)	2.952 (13)	132 (10)
O2W—H21W···O13	0.89 (12)	2.16 (12)	2.850 (10)	134 (12)
O12—H12···O13^vi	0.88 (5)	2.00 (12)	2.567 (13)	121 (12)
N4—H41···O1W^xi	0.83 (14)	2.12 (15)	2.928 (15)	164 (9)
N4—H42···O13^xii	0.91 (14)	2.20 (14)	3.082 (13)	166 (15)

Symmetry codes: (vi) x, −y+1, z+1/2; (x) −x+3/2, −y+3/2, z−1/2; (xi) −x+3/2, y−1/2, z; (xii) −x+3/2, −y+3/2, z+1/2.

Acknowledgements

The authors acknowledge support from the Science and Engineering Faculty, Queensland University of Technology and from Griffith University.

References

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Volume 73| Part 2| February 2017| Pages 203-208

https://doi.org/10.1107/S2056989017000445

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research communications\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Crystal structures and hydrogen bonding in the isotypic series of hydrated alkali metal (K, Rb and Cs) complexes with 4-amino­phenyl­arsonic acid

1. Chemical context

2. Structural commentary

3. Supra­molecular features

4. Database survey

5. Synthesis and crystallization

6. Refinement details

Supporting information

Acknowledgements

References

research communications

Crystal structures and hydrogen bonding in the isotypic series of hydrated alkali metal (K, Rb and Cs) complexes with 4-aminophenylarsonic acid

3. Supramolecular features