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

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

p-Arsanilic acid forms an isotypic set of three compounds with the alkali metals K, Rb and Cs, in which the primary layered coordination polymeric structures have similar asymmetric units comprising two independent and different metal cations and a bridging water molecule which lie within crystallographic mirror planes parallel to (100). The 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.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989017000445/wm5350sup1.cif Contains datablocks global, I, II, III
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989017000445/wm5350Isup2.hkl Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989017000445/wm5350IIsup3.hkl Contains datablock II
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989017000445/wm5350IIIsup4.hkl Contains datablock III

CCDC references: 1526425; 1526424; 1526423

checkCIF report

Key indicators

Structure: I

Single-crystal X-ray study
T = 200 K
Mean (C-C) = 0.008 Å
R factor = 0.030
wR factor = 0.125
Data-to-parameter ratio = 12.6

Structure: II

Single-crystal X-ray study
T = 200 K
Mean (C-C) = 0.007 Å
R factor = 0.032
wR factor = 0.072
Data-to-parameter ratio = 14.3

Structure: III

Single-crystal X-ray study
T = 200 K
Mean (C-C) = 0.016 Å
R factor = 0.041
wR factor = 0.160
Data-to-parameter ratio = 13.0

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level B
PLAT417_ALERT_2_B Short Inter D-H..H-D       H11W   ..  H42     ..       2.08 Ang.
PLAT915_ALERT_3_B No Flack x Check Done: Low Friedel Pair Coverage         44 %
PLAT934_ALERT_3_B Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          4 Check

Alert level C
PLAT213_ALERT_2_C Atom C4              has ADP max/min Ratio .....        3.1 oblate
PLAT341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00833 Ang.
PLAT918_ALERT_3_C Reflection(s) with I(obs) much Smaller I(calc) .          3 Check
PLAT939_ALERT_3_C Large Value of Not (SHELXL) Weight Optimized S .      38.90 Check
PLAT977_ALERT_2_C Check the Negative Difference Density on      H5      -0.36 eA-3
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Note

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         10 Note
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          2 Info
PLAT005_ALERT_5_G No Embedded Refinement Details found  in the CIF     Please Do !
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............          8 Note
PLAT899_ALERT_4_G SHELXL97   is Deprecated and Succeeded by SHELXL       2014 Note
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min)           2 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        193 Note

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

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




Datablock: II


Alert level C
PLAT341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00683 Ang.
PLAT910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min)           5 Note
PLAT915_ALERT_3_C No Flack x Check Done: Low Friedel Pair Coverage         57 %
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Note

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         10 Note
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          2 Info
PLAT005_ALERT_5_G No Embedded Refinement Details found  in the CIF     Please Do !
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............          8 Note
PLAT899_ALERT_4_G SHELXL97   is Deprecated and Succeeded by SHELXL       2014 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        159 Note

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

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




Datablock: III



Alert level B
PLAT915_ALERT_3_B No Flack x Check Done: Low Friedel Pair Coverage         30 %
PLAT934_ALERT_3_B Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          7 Check
PLAT973_ALERT_2_B Check Calcd Positive Residual Density on     Cs2       1.62 eA-3

Alert level C
PLAT342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.01633 Ang.
PLAT918_ALERT_3_C Reflection(s) with I(obs) much Smaller I(calc) .          6 Check
PLAT939_ALERT_3_C Large Value of Not (SHELXL) Weight Optimized S .      51.33 Check
PLAT975_ALERT_2_C Check Calcd Residual Density  0.53A From     O11       0.64 eA-3
PLAT975_ALERT_2_C Check Calcd Residual Density  1.03A From     O11       0.57 eA-3
PLAT975_ALERT_2_C Check Calcd Residual Density  0.74A From     O2W       0.56 eA-3
PLAT976_ALERT_2_C Check Calcd Residual Density  0.82A From     O1W      -0.99 eA-3
PLAT976_ALERT_2_C Check Calcd Residual Density  0.61A From     O1W      -0.95 eA-3
PLAT976_ALERT_2_C Check Calcd Residual Density  0.74A From     O2W      -0.67 eA-3
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Note

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         10 Note
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          2 Info
PLAT005_ALERT_5_G No Embedded Refinement Details found  in the CIF     Please Do !
PLAT072_ALERT_2_G SHELXL First  Parameter in WGHT  Unusually Large       0.12 Report
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............          8 Note
PLAT899_ALERT_4_G SHELXL97   is Deprecated and Succeeded by SHELXL       2014 Note
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min)           2 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        153 Note

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

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

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.

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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

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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