Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S205322961303338X/fn3158sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S205322961303338X/fn3158Cs2HAsO4.2H2Osup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S205322961303338X/fn3158Cs2HPO4.2H2Osup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S205322961303338X/fn3158Rb2HAsO4.2H2Osup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S205322961303338X/fn3158Rb2HPO4.2H2Osup5.hkl | |
Text file https://doi.org/10.1107/S205322961303338X/fn3158sup6.txt | |
Text file https://doi.org/10.1107/S205322961303338X/fn3158sup7.txt | |
Text file https://doi.org/10.1107/S205322961303338X/fn3158sup8.txt | |
Text file https://doi.org/10.1107/S205322961303338X/fn3158sup9.txt |
CCDC references: 976157; 976158; 976159; 976160
For all compounds, data collection: APEX2 (Bruker, 2013); cell refinement: SAINT-Plus (Bruker, 2013); data reduction: SAINT-Plus (Bruker, 2013). Program(s) used to solve structure: coordinates of Rb2HAsO4.2H2O for Cs2HAsO4.2H2O, Cs2HPO4.2H2O, Rb2HPO4.2H2O; SUPERFLIP (Palatinus & Chapuis, 2007) for Rb2HAsO4.2H2O. Program(s) used to refine structure: JANA2006 (Petříček et al., 2006) for Cs2HAsO4.2H2O, Cs2HPO4.2H2O, Rb2HPO4.2H2O; Jana2006 (Petříček et al., 2006) for Rb2HAsO4.2H2O. For all compounds, molecular graphics: ATOMS (Dowty, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).
Cs2HAsO4·2H2O | F(000) = 784 |
Mr = 441.8 | Dx = 3.694 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 9992 reflections |
a = 7.7015 (3) Å | θ = 2.9–32.6° |
b = 14.3265 (5) Å | µ = 13.29 mm−1 |
c = 8.1324 (3) Å | T = 100 K |
β = 117.7412 (14)° | Plate, clear colourless |
V = 794.16 (5) Å3 | 0.08 × 0.03 × 0.01 mm |
Z = 4 |
Bruker Kappa APEXII CCD diffractometer | 2895 independent reflections |
Radiation source: X-ray tube | 2452 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.039 |
ω and φ scans | θmax = 32.6°, θmin = 2.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2013) | h = −11→11 |
Tmin = 0.63, Tmax = 0.88 | k = −21→21 |
29263 measured reflections | l = −12→12 |
Refinement on F | Hydrogen site location: difference Fourier map |
R[F > 3σ(F)] = 0.015 | All H-atom parameters refined |
wR(F) = 0.025 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
S = 1.36 | (Δ/σ)max = 0.036 |
2895 reflections | Δρmax = 0.61 e Å−3 |
103 parameters | Δρmin = −0.66 e Å−3 |
7 restraints | Extinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974) |
0 constraints | Extinction coefficient: 660 (20) |
Primary atom site location: isomorphous structure methods |
x | y | z | Uiso*/Ueq | ||
Cs1 | 0.741813 (13) | 0.731792 (8) | 0.746055 (13) | 0.00784 (5) | |
Cs2 | 0.251517 (13) | 0.920139 (7) | 0.747393 (13) | 0.00975 (6) | |
As | 0.25340 (2) | 0.858572 (13) | 0.25900 (2) | 0.00545 (7) | |
O1 | 0.13398 (18) | 0.79315 (9) | 0.05609 (18) | 0.0133 (5) | |
O2 | 0.42685 (19) | 0.92271 (7) | 0.2428 (2) | 0.0107 (5) | |
O3 | 0.35337 (18) | 0.78242 (8) | 0.43520 (18) | 0.0124 (5) | |
O4 | 0.07415 (19) | 0.92168 (8) | 0.2658 (2) | 0.0105 (5) | |
Ow1 | 0.7871 (2) | 0.91323 (9) | 0.5508 (2) | 0.0123 (5) | |
Ow2 | 0.7157 (2) | 0.58410 (9) | 0.4535 (2) | 0.0117 (5) | |
Hw21 | 0.8315 (17) | 0.592 (2) | 0.541 (3) | 0.086 (15)* | |
Hw11 | 0.673 (2) | 0.911 (2) | 0.458 (3) | 0.100 (17)* | |
H1 | 0.221 (3) | 0.7699 (18) | 0.032 (5) | 0.094 (13)* | |
Hw12 | 0.824 (4) | 0.9553 (14) | 0.634 (3) | 0.054 (10)* | |
Hw22 | 0.683 (4) | 0.5406 (15) | 0.374 (3) | 0.061 (11)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cs1 | 0.00774 (7) | 0.00726 (6) | 0.00649 (6) | −0.00023 (3) | 0.00161 (5) | 0.00015 (3) |
Cs2 | 0.00932 (8) | 0.00756 (7) | 0.01131 (7) | 0.00009 (3) | 0.00390 (6) | 0.00026 (3) |
As | 0.00500 (9) | 0.00517 (9) | 0.00524 (9) | −0.00006 (5) | 0.00160 (7) | 0.00016 (5) |
O1 | 0.0083 (6) | 0.0175 (6) | 0.0106 (6) | −0.0005 (5) | 0.0014 (5) | −0.0075 (5) |
O2 | 0.0083 (6) | 0.0104 (6) | 0.0134 (6) | −0.0009 (4) | 0.0051 (5) | 0.0025 (4) |
O3 | 0.0101 (6) | 0.0126 (6) | 0.0113 (6) | 0.0014 (4) | 0.0024 (5) | 0.0077 (4) |
O4 | 0.0079 (6) | 0.0106 (6) | 0.0131 (6) | 0.0011 (4) | 0.0048 (5) | −0.0026 (4) |
Ow1 | 0.0104 (6) | 0.0116 (6) | 0.0122 (6) | −0.0002 (5) | 0.0030 (5) | −0.0025 (5) |
Ow2 | 0.0093 (6) | 0.0103 (6) | 0.0127 (6) | 0.0003 (4) | 0.0027 (5) | −0.0030 (4) |
Cs1—O1i | 3.0269 (11) | Cs2—O3 | 3.5789 (16) |
Cs1—O2ii | 3.2748 (14) | Cs2—O3ii | 3.2022 (12) |
Cs1—O3 | 2.9708 (11) | Cs2—O4 | 3.4963 (15) |
Cs1—O4iii | 3.3209 (14) | Cs2—O4vi | 3.3447 (14) |
Cs1—Ow1 | 3.1489 (16) | Cs2—Ow1vii | 3.1677 (15) |
Cs1—Ow1ii | 3.1266 (16) | Cs2—Ow1v | 3.3161 (16) |
Cs1—Ow2 | 3.1194 (16) | Cs2—Ow2viii | 3.3053 (16) |
Cs1—Ow2ii | 3.1876 (15) | Cs2—Ow2ii | 3.1643 (14) |
Cs2—O1iv | 3.5422 (16) | As—O1 | 1.7420 (13) |
Cs2—O1ii | 3.3565 (13) | As—O2 | 1.6764 (16) |
Cs2—O2iv | 3.6043 (16) | As—O3 | 1.6761 (12) |
Cs2—O2v | 3.3206 (14) | As—O4 | 1.6725 (15) |
O1i—Cs1—O2ii | 130.63 (4) | O2iv—Cs2—O3 | 134.98 (3) |
O1i—Cs1—O3 | 148.98 (3) | O2iv—Cs2—O3ii | 66.11 (3) |
O1i—Cs1—O4iii | 72.80 (3) | O2iv—Cs2—O4 | 178.72 (3) |
O1i—Cs1—Ow1 | 83.02 (3) | O2iv—Cs2—O4vi | 85.07 (3) |
O1i—Cs1—Ow1ii | 80.37 (4) | O2iv—Cs2—Ow1vii | 108.18 (4) |
O1i—Cs1—Ow2 | 121.16 (4) | O2iv—Cs2—Ow1v | 132.02 (3) |
O1i—Cs1—Ow2ii | 66.62 (4) | O2iv—Cs2—Ow2viii | 46.35 (3) |
O2ii—Cs1—O3 | 73.11 (3) | O2iv—Cs2—Ow2ii | 70.42 (4) |
O2ii—Cs1—O4iii | 95.98 (3) | O2v—Cs2—O3 | 89.05 (4) |
O2ii—Cs1—Ow1 | 144.04 (3) | O2v—Cs2—O3ii | 126.06 (3) |
O2ii—Cs1—Ow1ii | 50.67 (3) | O2v—Cs2—O4 | 85.46 (3) |
O2ii—Cs1—Ow2 | 75.56 (4) | O2v—Cs2—O4vi | 94.66 (3) |
O2ii—Cs1—Ow2ii | 109.54 (4) | O2v—Cs2—Ow1vii | 133.45 (3) |
O3—Cs1—O4iii | 130.61 (4) | O2v—Cs2—Ow1v | 48.81 (3) |
O3—Cs1—Ow1 | 70.94 (4) | O2v—Cs2—Ow2viii | 72.53 (4) |
O3—Cs1—Ow1ii | 122.23 (4) | O2v—Cs2—Ow2ii | 49.77 (3) |
O3—Cs1—Ow2 | 80.48 (4) | O3—Cs2—O3ii | 75.69 (4) |
O3—Cs1—Ow2ii | 87.80 (3) | O3—Cs2—O4 | 46.31 (3) |
O4iii—Cs1—Ow1 | 107.89 (4) | O3—Cs2—O4vi | 139.42 (3) |
O4iii—Cs1—Ow1ii | 73.89 (4) | O3—Cs2—Ow1vii | 101.16 (4) |
O4iii—Cs1—Ow2 | 50.40 (3) | O3—Cs2—Ow1v | 81.53 (4) |
O4iii—Cs1—Ow2ii | 139.41 (3) | O3—Cs2—Ow2viii | 161.24 (4) |
Ow1—Cs1—Ow1ii | 161.91 (3) | O3—Cs2—Ow2ii | 78.39 (4) |
Ow1—Cs1—Ow2 | 99.11 (4) | O3ii—Cs2—O4 | 114.91 (3) |
Ow1—Cs1—Ow2ii | 68.47 (5) | O3ii—Cs2—O4vi | 130.01 (4) |
Ow1ii—Cs1—Ow2 | 95.60 (4) | O3ii—Cs2—Ow1vii | 100.41 (3) |
Ow1ii—Cs1—Ow2ii | 98.13 (4) | O3ii—Cs2—Ow1v | 156.91 (4) |
Ow2—Cs1—Ow2ii | 165.33 (4) | O3ii—Cs2—Ow2viii | 112.04 (4) |
O1iv—Cs2—O1ii | 76.00 (4) | O3ii—Cs2—Ow2ii | 76.37 (3) |
O1iv—Cs2—O2iv | 45.53 (3) | O4—Cs2—O4vi | 93.65 (3) |
O1iv—Cs2—O2v | 139.91 (3) | O4—Cs2—Ow1vii | 70.99 (4) |
O1iv—Cs2—O3 | 115.62 (3) | O4—Cs2—Ow1v | 47.24 (3) |
O1iv—Cs2—O3ii | 44.21 (4) | O4—Cs2—Ow2viii | 132.53 (3) |
O1iv—Cs2—O4 | 134.56 (3) | O4—Cs2—Ow2ii | 110.46 (4) |
O1iv—Cs2—O4vi | 86.30 (4) | O4vi—Cs2—Ow1vii | 49.56 (3) |
O1iv—Cs2—Ow1vii | 74.97 (4) | O4vi—Cs2—Ow1v | 71.22 (4) |
O1iv—Cs2—Ow1v | 157.29 (4) | O4vi—Cs2—Ow2viii | 48.81 (3) |
O1iv—Cs2—Ow2viii | 78.51 (4) | O4vi—Cs2—Ow2ii | 132.48 (3) |
O1iv—Cs2—Ow2ii | 102.30 (4) | Ow1vii—Cs2—Ow1v | 87.57 (4) |
O1ii—Cs2—O2iv | 114.04 (3) | Ow1vii—Cs2—Ow2viii | 94.32 (4) |
O1ii—Cs2—O2v | 131.73 (4) | Ow1vii—Cs2—Ow2ii | 176.78 (4) |
O1ii—Cs2—O3 | 43.13 (4) | Ow1v—Cs2—Ow2viii | 88.66 (4) |
O1ii—Cs2—O3ii | 49.41 (3) | Ow1v—Cs2—Ow2ii | 95.51 (4) |
O1ii—Cs2—O4 | 66.80 (3) | Ow2viii—Cs2—Ow2ii | 86.74 (4) |
O1ii—Cs2—O4vi | 124.44 (3) | O1—As—O2 | 108.01 (8) |
O1ii—Cs2—Ow1vii | 74.93 (3) | O1—As—O3 | 106.83 (6) |
O1ii—Cs2—Ow1v | 113.79 (4) | O1—As—O4 | 104.02 (6) |
O1ii—Cs2—Ow2viii | 154.13 (4) | O2—As—O3 | 110.99 (6) |
O1ii—Cs2—Ow2ii | 102.86 (3) | O3—As—O4 | 112.42 (8) |
O2iv—Cs2—O2v | 94.53 (3) |
Symmetry codes: (i) x+1, y, z+1; (ii) x, −y+3/2, z+1/2; (iii) x+1, −y+3/2, z+1/2; (iv) x, y, z+1; (v) −x+1, −y+2, −z+1; (vi) −x, −y+2, −z+1; (vii) x−1, y, z; (viii) −x+1, y+1/2, −z+3/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O3ix | 0.85 (3) | 1.72 (4) | 2.557 (2) | 167 (3) |
Ow1—Hw11···O2 | 0.850 (15) | 1.897 (16) | 2.7425 (17) | 172 (3) |
Ow1—Hw12···O4v | 0.85 (2) | 1.95 (2) | 2.7343 (17) | 153 (3) |
Ow2—Hw21···O4iii | 0.850 (13) | 1.922 (16) | 2.7480 (17) | 164 (3) |
Ow2—Hw22···O2x | 0.85 (2) | 1.93 (2) | 2.7328 (17) | 158 (3) |
Symmetry codes: (iii) x+1, −y+3/2, z+1/2; (v) −x+1, −y+2, −z+1; (ix) x, −y+3/2, z−1/2; (x) −x+1, y−1/2, −z+1/2. |
Cs2HPO4·2H2O | F(000) = 712 |
Mr = 397.8 | Dx = 3.510 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 9974 reflections |
a = 7.4764 (5) Å | θ = 2.9–32.6° |
b = 14.1898 (10) Å | µ = 9.87 mm−1 |
c = 7.9535 (6) Å | T = 100 K |
β = 116.880 (2)° | Plate, clear colourless |
V = 752.61 (9) Å3 | 0.05 × 0.04 × 0.01 mm |
Z = 4 |
Bruker Kappa APEXII CCD diffractometer | 2756 independent reflections |
Radiation source: X-ray tube | 2503 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.050 |
ω and φ scans | θmax = 32.6°, θmin = 2.9° |
Absorption correction: multi-scan (SADABS; Bruker, 2013) | h = −11→11 |
Tmin = 0.63, Tmax = 0.90 | k = −21→21 |
25736 measured reflections | l = −12→12 |
Refinement on F | Hydrogen site location: difference Fourier map |
R[F > 3σ(F)] = 0.020 | All H-atom parameters refined |
wR(F) = 0.033 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
S = 1.61 | (Δ/σ)max = 0.030 |
2756 reflections | Δρmax = 0.88 e Å−3 |
101 parameters | Δρmin = −0.65 e Å−3 |
5 restraints | Extinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974) |
2 constraints | Extinction coefficient: 1410 (50) |
Primary atom site location: isomorphous structure methods |
x | y | z | Uiso*/Ueq | ||
Cs1 | 0.742006 (15) | 0.731846 (10) | 0.746496 (12) | 0.00725 (6) | |
Cs2 | 0.251965 (13) | 0.918915 (9) | 0.745719 (13) | 0.00898 (7) | |
P | 0.25330 (5) | 0.85516 (4) | 0.25943 (5) | 0.00527 (16) | |
O1 | 0.1409 (2) | 0.79501 (10) | 0.06896 (18) | 0.0112 (4) | |
O2 | 0.4132 (2) | 0.91487 (9) | 0.2418 (2) | 0.0093 (5) | |
O3 | 0.3467 (2) | 0.78525 (9) | 0.42224 (18) | 0.0114 (5) | |
O4 | 0.0879 (2) | 0.91339 (9) | 0.2696 (2) | 0.0096 (5) | |
Ow1 | 0.7811 (3) | 0.91652 (10) | 0.5516 (2) | 0.0118 (5) | |
Ow2 | 0.7218 (3) | 0.58033 (9) | 0.4544 (2) | 0.0114 (5) | |
Hw22 | 0.688 (4) | 0.5330 (12) | 0.381 (3) | 0.023 (6)* | |
Hw12 | 0.816 (4) | 0.9668 (11) | 0.617 (3) | 0.027 (6)* | |
Hw21 | 0.8430 (16) | 0.5766 (17) | 0.538 (3) | 0.023 (6)* | |
Hw11 | 0.665 (2) | 0.9235 (17) | 0.460 (3) | 0.027 (6)* | |
H1 | 0.218 (3) | 0.7729 (17) | 0.027 (3) | 0.053 (10)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cs1 | 0.00793 (9) | 0.00672 (9) | 0.00628 (8) | −0.00014 (3) | 0.00250 (6) | 0.00015 (3) |
Cs2 | 0.00966 (10) | 0.00689 (10) | 0.00979 (9) | 0.00009 (3) | 0.00388 (8) | 0.00017 (3) |
P | 0.0061 (2) | 0.0042 (2) | 0.00535 (19) | −0.00004 (12) | 0.00243 (18) | 0.00013 (12) |
O1 | 0.0107 (6) | 0.0124 (6) | 0.0097 (6) | −0.0013 (5) | 0.0038 (5) | −0.0051 (5) |
O2 | 0.0094 (7) | 0.0079 (6) | 0.0118 (6) | −0.0003 (4) | 0.0057 (5) | 0.0024 (4) |
O3 | 0.0127 (6) | 0.0099 (6) | 0.0105 (6) | 0.0004 (5) | 0.0042 (5) | 0.0043 (4) |
O4 | 0.0103 (7) | 0.0080 (6) | 0.0107 (6) | 0.0010 (5) | 0.0049 (5) | −0.0024 (5) |
Ow1 | 0.0120 (7) | 0.0096 (7) | 0.0130 (7) | 0.0013 (5) | 0.0050 (6) | −0.0011 (4) |
Ow2 | 0.0108 (7) | 0.0095 (7) | 0.0130 (7) | 0.0004 (5) | 0.0045 (6) | −0.0026 (4) |
Cs1—O1i | 3.0595 (13) | Cs2—O3 | 3.5166 (17) |
Cs1—O2ii | 3.2088 (17) | Cs2—O3ii | 3.1570 (14) |
Cs1—O3 | 3.0112 (13) | Cs2—O4 | 3.4135 (16) |
Cs1—O4iii | 3.2464 (17) | Cs2—O4vi | 3.4429 (16) |
Cs1—Ow1 | 3.1249 (17) | Cs2—Ow1vii | 3.1408 (18) |
Cs1—Ow1ii | 3.1249 (18) | Cs2—Ow1v | 3.2522 (17) |
Cs1—Ow2 | 3.1186 (18) | Cs2—Ow2viii | 3.2482 (17) |
Cs1—Ow2ii | 3.1759 (16) | Cs2—Ow2ii | 3.1339 (18) |
Cs2—O1iv | 3.5098 (17) | P—O1 | 1.6057 (14) |
Cs2—O1ii | 3.2901 (15) | P—O2 | 1.5226 (18) |
Cs2—O2iv | 3.5671 (17) | P—O3 | 1.5267 (14) |
Cs2—O2v | 3.4081 (16) | P—O4 | 1.5195 (18) |
O1i—Cs1—O2ii | 130.63 (4) | O2iv—Cs2—O3 | 136.18 (3) |
O1i—Cs1—O3 | 148.38 (4) | O2iv—Cs2—O3ii | 66.28 (3) |
O1i—Cs1—O4iii | 71.87 (4) | O2iv—Cs2—O4 | 177.48 (3) |
O1i—Cs1—Ow1 | 84.02 (4) | O2iv—Cs2—O4vi | 85.70 (4) |
O1i—Cs1—Ow1ii | 80.39 (4) | O2iv—Cs2—Ow1vii | 106.66 (5) |
O1i—Cs1—Ow2 | 121.80 (4) | O2iv—Cs2—Ow1v | 133.82 (3) |
O1i—Cs1—Ow2ii | 64.88 (4) | O2iv—Cs2—Ow2viii | 47.24 (3) |
O2ii—Cs1—O3 | 72.74 (4) | O2iv—Cs2—Ow2ii | 71.15 (5) |
O2ii—Cs1—O4iii | 100.09 (4) | O2v—Cs2—O3 | 90.36 (4) |
O2ii—Cs1—Ow1 | 141.38 (4) | O2v—Cs2—O3ii | 127.44 (3) |
O2ii—Cs1—Ow1ii | 51.25 (4) | O2v—Cs2—O4 | 86.50 (4) |
O2ii—Cs1—Ow2 | 76.42 (5) | O2v—Cs2—O4vi | 92.49 (4) |
O2ii—Cs1—Ow2ii | 109.51 (5) | O2v—Cs2—Ow1vii | 131.85 (4) |
O3—Cs1—O4iii | 131.03 (4) | O2v—Cs2—Ow1v | 48.52 (3) |
O3—Cs1—Ow1 | 68.88 (4) | O2v—Cs2—Ow2viii | 72.00 (5) |
O3—Cs1—Ow1ii | 123.06 (4) | O2v—Cs2—Ow2ii | 49.42 (3) |
O3—Cs1—Ow2 | 80.63 (4) | O3—Cs2—O3ii | 75.61 (4) |
O3—Cs1—Ow2ii | 88.59 (4) | O3—Cs2—O4 | 42.79 (3) |
O4iii—Cs1—Ow1 | 108.04 (5) | O3—Cs2—O4vi | 137.43 (3) |
O4iii—Cs1—Ow1ii | 74.69 (5) | O3—Cs2—Ow1vii | 100.74 (4) |
O4iii—Cs1—Ow2 | 51.21 (4) | O3—Cs2—Ow1v | 80.18 (4) |
O4iii—Cs1—Ow2ii | 136.68 (4) | O3—Cs2—Ow2viii | 162.23 (4) |
Ow1—Cs1—Ow1ii | 162.42 (4) | O3—Cs2—Ow2ii | 80.85 (4) |
Ow1—Cs1—Ow2 | 101.10 (5) | O3ii—Cs2—O4 | 111.60 (3) |
Ow1—Cs1—Ow2ii | 65.90 (5) | O3ii—Cs2—O4vi | 131.57 (4) |
Ow1ii—Cs1—Ow2 | 94.02 (4) | O3ii—Cs2—Ow1vii | 100.66 (4) |
Ow1ii—Cs1—Ow2ii | 99.84 (5) | O3ii—Cs2—Ow1v | 155.54 (5) |
Ow2—Cs1—Ow2ii | 165.64 (4) | O3ii—Cs2—Ow2viii | 113.18 (4) |
O1iv—Cs2—O1ii | 75.72 (4) | O3ii—Cs2—Ow2ii | 78.18 (4) |
O1iv—Cs2—O2iv | 41.86 (3) | O4—Cs2—O4vi | 95.01 (4) |
O1iv—Cs2—O2v | 137.66 (3) | O4—Cs2—Ow1vii | 72.16 (5) |
O1iv—Cs2—O3 | 117.28 (3) | O4—Cs2—Ow1v | 48.61 (4) |
O1iv—Cs2—O3ii | 45.12 (4) | O4—Cs2—Ow2viii | 134.67 (3) |
O1iv—Cs2—O4 | 135.71 (3) | O4—Cs2—Ow2ii | 110.01 (5) |
O1iv—Cs2—O4vi | 87.53 (4) | O4vi—Cs2—Ow1vii | 49.06 (4) |
O1iv—Cs2—Ow1vii | 76.76 (4) | O4vi—Cs2—Ow1v | 70.48 (5) |
O1iv—Cs2—Ow1v | 157.95 (4) | O4vi—Cs2—Ow2viii | 48.49 (3) |
O1iv—Cs2—Ow2viii | 76.77 (4) | O4vi—Cs2—Ow2ii | 130.46 (3) |
O1iv—Cs2—Ow2ii | 101.15 (4) | Ow1vii—Cs2—Ow1v | 87.17 (4) |
O1ii—Cs2—O2iv | 110.59 (3) | Ow1vii—Cs2—Ow2viii | 92.91 (5) |
O1ii—Cs2—O2v | 133.71 (4) | Ow1vii—Cs2—Ow2ii | 177.78 (5) |
O1ii—Cs2—O3 | 44.37 (4) | Ow1v—Cs2—Ow2viii | 89.26 (4) |
O1ii—Cs2—O3ii | 46.04 (3) | Ow1v—Cs2—Ow2ii | 94.65 (4) |
O1ii—Cs2—O4 | 67.05 (3) | Ow2viii—Cs2—Ow2ii | 85.85 (4) |
O1ii—Cs2—O4vi | 125.66 (3) | O1—P—O2 | 107.85 (9) |
O1ii—Cs2—Ow1vii | 76.69 (4) | O1—P—O3 | 107.37 (8) |
O1ii—Cs2—Ow1v | 115.48 (4) | O1—P—O4 | 104.36 (7) |
O1ii—Cs2—Ow2viii | 152.15 (5) | O2—P—O3 | 111.25 (8) |
O1ii—Cs2—Ow2ii | 103.61 (4) | O3—P—O4 | 112.31 (9) |
O2iv—Cs2—O2v | 95.88 (4) |
Symmetry codes: (i) x+1, y, z+1; (ii) x, −y+3/2, z+1/2; (iii) x+1, −y+3/2, z+1/2; (iv) x, y, z+1; (v) −x+1, −y+2, −z+1; (vi) −x, −y+2, −z+1; (vii) x−1, y, z; (viii) −x+1, y+1/2, −z+3/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O3ix | 0.85 (3) | 1.74 (3) | 2.579 (2) | 171 (2) |
Ow1—Hw11···O2 | 0.850 (15) | 1.902 (15) | 2.7400 (19) | 169 (2) |
Ow1—Hw12···O4v | 0.850 (18) | 1.908 (17) | 2.747 (2) | 169 (3) |
Ow2—Hw21···O4iii | 0.850 (12) | 1.927 (16) | 2.753 (2) | 164 (3) |
Ow2—Hw22···O2x | 0.850 (19) | 1.915 (18) | 2.7461 (19) | 165 (3) |
Symmetry codes: (iii) x+1, −y+3/2, z+1/2; (v) −x+1, −y+2, −z+1; (ix) x, −y+3/2, z−1/2; (x) −x+1, y−1/2, −z+1/2. |
Rb2HAsO4·2H2O | F(000) = 640 |
Mr = 346.9 | Dx = 3.171 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 9969 reflections |
a = 7.6087 (5) Å | θ = 3.0–39.9° |
b = 13.7823 (3) Å | µ = 17.96 mm−1 |
c = 7.9260 (3) Å | T = 100 K |
β = 119.074 (6)° | Plate, clear colourless |
V = 726.43 (7) Å3 | 0.09 × 0.06 × 0.01 mm |
Z = 4 |
Bruker Kappa APEX II CCD diffractometer | 4510 independent reflections |
Radiation source: X-ray tube | 3170 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.032 |
ω and φ scans | θmax = 40.1°, θmin = 3.0° |
Absorption correction: multi-scan (SADABS; Bruker, 2013) | h = −12→13 |
Tmin = 0.29, Tmax = 0.84 | k = −24→24 |
34648 measured reflections | l = −14→13 |
Refinement on F | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.020 | All H-atom parameters refined |
wR(F2) = 0.027 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
S = 1.22 | (Δ/σ)max = 0.038 |
4510 reflections | Δρmax = 0.85 e Å−3 |
103 parameters | Δρmin = −0.82 e Å−3 |
7 restraints | Extinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974) |
0 constraints | Extinction coefficient: 320 (30) |
Primary atom site location: iterative |
x | y | z | Uiso*/Ueq | ||
Rb1 | 0.742563 (17) | 0.734776 (10) | 0.750523 (15) | 0.01081 (4) | |
Rb2 | 0.253648 (17) | 0.920312 (10) | 0.745047 (16) | 0.01417 (5) | |
As | 0.256241 (17) | 0.858760 (10) | 0.257834 (15) | 0.00787 (4) | |
O1 | 0.13025 (15) | 0.79310 (9) | 0.04544 (14) | 0.0212 (4) | |
O2 | 0.43131 (14) | 0.92581 (7) | 0.24367 (14) | 0.0139 (3) | |
O3 | 0.36431 (15) | 0.77792 (8) | 0.43771 (15) | 0.0203 (4) | |
O4 | 0.07583 (14) | 0.92162 (7) | 0.27102 (14) | 0.0136 (3) | |
Ow1 | 0.80300 (15) | 0.90481 (8) | 0.55311 (15) | 0.0142 (4) | |
Ow2 | 0.70292 (15) | 0.59131 (8) | 0.45985 (15) | 0.0151 (4) | |
Hw11 | 0.6880 (17) | 0.8973 (16) | 0.454 (3) | 0.124 (13)* | |
Hw22 | 0.668 (3) | 0.5454 (10) | 0.378 (2) | 0.029 (6)* | |
Hw12 | 0.837 (3) | 0.9551 (8) | 0.624 (2) | 0.023 (5)* | |
Hw21 | 0.8244 (9) | 0.6043 (17) | 0.541 (3) | 0.095 (10)* | |
H1 | 0.223 (2) | 0.7724 (16) | 0.025 (3) | 0.093 (10)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Rb1 | 0.01071 (6) | 0.00994 (6) | 0.00939 (6) | −0.00045 (4) | 0.00301 (4) | 0.00030 (4) |
Rb2 | 0.01171 (6) | 0.01029 (6) | 0.01747 (7) | −0.00014 (5) | 0.00468 (5) | 0.00033 (5) |
As | 0.00700 (6) | 0.00742 (6) | 0.00797 (6) | −0.00014 (5) | 0.00268 (4) | 0.00015 (5) |
O1 | 0.0118 (5) | 0.0287 (7) | 0.0196 (5) | −0.0029 (4) | 0.0049 (4) | −0.0149 (5) |
O2 | 0.0100 (4) | 0.0139 (5) | 0.0171 (5) | −0.0016 (3) | 0.0060 (4) | 0.0041 (4) |
O3 | 0.0137 (5) | 0.0206 (6) | 0.0223 (5) | 0.0017 (4) | 0.0053 (4) | 0.0144 (4) |
O4 | 0.0108 (4) | 0.0136 (5) | 0.0166 (5) | 0.0005 (3) | 0.0067 (4) | −0.0036 (4) |
Ow1 | 0.0121 (4) | 0.0124 (5) | 0.0156 (4) | 0.0002 (3) | 0.0047 (4) | −0.0035 (4) |
Ow2 | 0.0108 (4) | 0.0154 (5) | 0.0166 (5) | −0.0002 (3) | 0.0047 (4) | −0.0047 (4) |
Rb1—O1i | 2.8478 (10) | Rb2—O3 | 3.5337 (13) |
Rb1—O2ii | 3.2226 (11) | Rb2—O3ii | 3.0423 (11) |
Rb1—O3 | 2.8016 (10) | Rb2—O4 | 3.3176 (11) |
Rb1—O4iii | 3.2714 (11) | Rb2—O4vi | 3.2767 (11) |
Rb1—Ow1 | 2.9750 (12) | Rb2—Ow1vii | 3.0079 (12) |
Rb1—Ow1ii | 2.9313 (12) | Rb2—Ow1v | 3.2542 (11) |
Rb1—Ow2 | 2.9382 (12) | Rb2—Ow2viii | 3.2223 (12) |
Rb1—Ow2ii | 3.0125 (12) | Rb2—Ow2ii | 2.9922 (12) |
Rb2—O1iv | 3.4346 (13) | As—O1 | 1.7330 (11) |
Rb2—O1ii | 3.2546 (12) | As—O2 | 1.6692 (12) |
Rb2—O2iv | 3.5015 (11) | As—O3 | 1.6765 (10) |
Rb2—O2v | 3.1691 (11) | As—O4 | 1.6689 (12) |
O1i—Rb1—O2ii | 131.86 (3) | O2iv—Rb2—O2v | 94.69 (3) |
O1i—Rb1—O3 | 151.09 (3) | O2iv—Rb2—O3 | 134.38 (2) |
O1i—Rb1—O4iii | 71.13 (3) | O2iv—Rb2—O3ii | 65.92 (3) |
O1i—Rb1—Ow1 | 81.15 (3) | O2iv—Rb2—O4 | 178.06 (2) |
O1i—Rb1—Ow1ii | 79.96 (3) | O2iv—Rb2—O4vi | 84.14 (3) |
O1i—Rb1—Ow2 | 120.28 (3) | O2iv—Rb2—Ow1vii | 107.00 (3) |
O1i—Rb1—Ow2ii | 70.39 (3) | O2iv—Rb2—Ow1v | 130.23 (2) |
O2ii—Rb1—O3 | 72.56 (3) | O2iv—Rb2—Ow2viii | 46.98 (2) |
O2ii—Rb1—O4iii | 95.39 (3) | O2iv—Rb2—Ow2ii | 69.59 (3) |
O2ii—Rb1—Ow1 | 146.33 (2) | O2v—Rb2—O3 | 87.75 (3) |
O2ii—Rb1—Ow1ii | 52.04 (2) | O2v—Rb2—O3ii | 124.45 (3) |
O2ii—Rb1—Ow2 | 74.34 (3) | O2v—Rb2—O4 | 85.12 (3) |
O2ii—Rb1—Ow2ii | 106.64 (3) | O2v—Rb2—O4vi | 96.32 (3) |
O3—Rb1—O4iii | 128.46 (3) | O2v—Rb2—Ow1vii | 136.26 (3) |
O3—Rb1—Ow1 | 73.87 (3) | O2v—Rb2—Ow1v | 49.93 (2) |
O3—Rb1—Ow1ii | 123.27 (3) | O2v—Rb2—Ow2viii | 71.38 (3) |
O3—Rb1—Ow2 | 77.23 (3) | O2v—Rb2—Ow2ii | 51.72 (3) |
O3—Rb1—Ow2ii | 89.07 (3) | O3—Rb2—O3ii | 75.33 (3) |
O4iii—Rb1—Ow1 | 103.35 (3) | O3—Rb2—O4 | 47.55 (2) |
O4iii—Rb1—Ow1ii | 73.58 (3) | O3—Rb2—O4vi | 140.94 (2) |
O4iii—Rb1—Ow2 | 51.49 (2) | O3—Rb2—Ow1vii | 101.94 (3) |
O4iii—Rb1—Ow2ii | 141.22 (2) | O3—Rb2—Ow1v | 84.41 (3) |
Ow1—Rb1—Ow1ii | 160.80 (2) | O3—Rb2—Ow2viii | 158.72 (3) |
Ow1—Rb1—Ow2 | 95.79 (3) | O3—Rb2—Ow2ii | 76.91 (3) |
Ow1—Rb1—Ow2ii | 75.25 (3) | O3ii—Rb2—O4 | 115.75 (3) |
Ow1ii—Rb1—Ow2 | 96.63 (3) | O3ii—Rb2—O4vi | 129.53 (3) |
Ow1ii—Rb1—Ow2ii | 95.13 (3) | O3ii—Rb2—Ow1vii | 99.18 (3) |
Ow2—Rb1—Ow2ii | 165.39 (3) | O3ii—Rb2—Ow1v | 159.44 (4) |
O1iv—Rb2—O1ii | 76.36 (3) | O3ii—Rb2—Ow2viii | 112.75 (3) |
O1iv—Rb2—O2iv | 46.71 (2) | O3ii—Rb2—Ow2ii | 72.86 (3) |
O1iv—Rb2—O2v | 141.25 (2) | O4—Rb2—O4vi | 93.96 (3) |
O1iv—Rb2—O3 | 115.55 (3) | O4—Rb2—Ow1vii | 71.96 (3) |
O1iv—Rb2—O3ii | 45.24 (3) | O4—Rb2—Ow1v | 48.42 (2) |
O1iv—Rb2—O4 | 133.58 (2) | O4—Rb2—Ow2viii | 131.27 (3) |
O1iv—Rb2—O4vi | 84.53 (3) | O4—Rb2—Ow2ii | 111.66 (3) |
O1iv—Rb2—Ow1vii | 71.69 (3) | O4vi—Rb2—Ow1vii | 50.58 (3) |
O1iv—Rb2—Ow1v | 153.78 (3) | O4vi—Rb2—Ow1v | 69.54 (3) |
O1iv—Rb2—Ow2viii | 80.58 (3) | O4vi—Rb2—Ow2viii | 49.35 (2) |
O1iv—Rb2—Ow2ii | 101.52 (3) | O4vi—Rb2—Ow2ii | 134.32 (3) |
O1ii—Rb2—O2iv | 115.48 (3) | Ow1vii—Rb2—Ow1v | 88.23 (3) |
O1ii—Rb2—O2v | 130.85 (3) | Ow1vii—Rb2—Ow2viii | 96.24 (3) |
O1ii—Rb2—O3 | 43.29 (3) | Ow1vii—Rb2—Ow2ii | 172.02 (3) |
O1ii—Rb2—O3ii | 51.43 (3) | Ow1v—Rb2—Ow2viii | 85.19 (3) |
O1ii—Rb2—O4 | 65.91 (3) | Ow2viii—Rb2—Ow2ii | 86.58 (3) |
O1ii—Rb2—O4vi | 123.19 (3) | O1—As—O2 | 107.85 (6) |
O1ii—Rb2—Ow1vii | 72.62 (3) | O1—As—O3 | 106.88 (5) |
O1ii—Rb2—Ow1v | 114.28 (3) | O1—As—O4 | 104.38 (5) |
O1ii—Rb2—Ow2viii | 156.56 (3) | O2—As—O3 | 110.33 (5) |
O1ii—Rb2—Ow2ii | 102.01 (3) | O3—As—O4 | 111.73 (6) |
Symmetry codes: (i) x+1, y, z+1; (ii) x, −y+3/2, z+1/2; (iii) x+1, −y+3/2, z+1/2; (iv) x, y, z+1; (v) −x+1, −y+2, −z+1; (vi) −x, −y+2, −z+1; (vii) x−1, y, z; (viii) −x+1, y+1/2, −z+3/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O3ix | 0.85 (2) | 1.68 (2) | 2.5173 (19) | 167.3 (17) |
Ow1—Hw11···O2 | 0.850 (12) | 1.894 (12) | 2.7122 (13) | 161 (2) |
Ow1—Hw12···O4v | 0.850 (12) | 1.866 (11) | 2.6957 (14) | 165.0 (19) |
Ow2—Hw21···O4iii | 0.850 (9) | 1.929 (12) | 2.7137 (13) | 153 (2) |
Ow2—Hw22···O2x | 0.850 (14) | 1.873 (13) | 2.6920 (14) | 161.3 (19) |
Symmetry codes: (iii) x+1, −y+3/2, z+1/2; (v) −x+1, −y+2, −z+1; (ix) x, −y+3/2, z−1/2; (x) −x+1, y−1/2, −z+1/2. |
Rb2HPO4·2H2O | F(000) = 568 |
Mr = 302.9 | Dx = 2.935 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 9938 reflections |
a = 7.3640 (7) Å | θ = 3.0–32.7° |
b = 13.6496 (13) Å | µ = 14.48 mm−1 |
c = 7.7341 (8) Å | T = 100 K |
β = 118.176 (2)° | Plate, clear colourless |
V = 685.28 (12) Å3 | 0.11 × 0.08 × 0.01 mm |
Z = 4 |
Bruker Kappa APEXII CCD diffractometer | 2521 independent reflections |
Radiation source: X-ray tube | 2082 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.060 |
ω and φ scans | θmax = 32.7°, θmin = 3.0° |
Absorption correction: multi-scan (SADABS; Bruker, 2013) | h = −11→11 |
Tmin = 0.26, Tmax = 0.87 | k = −20→20 |
31969 measured reflections | l = −11→11 |
Refinement on F | Hydrogen site location: difference Fourier map |
R[F > 3σ(F)] = 0.030 | All H-atom parameters refined |
wR(F) = 0.039 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
S = 1.87 | (Δ/σ)max = 0.027 |
2521 reflections | Δρmax = 2.11 e Å−3 |
103 parameters | Δρmin = −1.57 e Å−3 |
4 restraints | Extinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974) |
0 constraints | Extinction coefficient: 670 (70) |
Primary atom site location: isomorphous structure methods |
x | y | z | Uiso*/Ueq | ||
Rb1 | 0.75415 (3) | 0.734074 (18) | 0.75918 (4) | 0.00688 (10) | |
Rb2 | 0.26528 (4) | 0.918714 (18) | 0.74357 (4) | 0.00941 (10) | |
P | 0.26995 (10) | 0.85369 (5) | 0.26065 (10) | 0.0047 (2) | |
O1 | 0.1533 (3) | 0.79367 (15) | 0.0608 (3) | 0.0112 (7) | |
O2 | 0.4268 (3) | 0.91989 (13) | 0.2439 (3) | 0.0088 (7) | |
O3 | 0.3772 (3) | 0.77962 (14) | 0.4260 (3) | 0.0110 (7) | |
O4 | 0.1007 (3) | 0.90850 (13) | 0.2795 (3) | 0.0087 (7) | |
Ow1 | 0.8083 (3) | 0.91058 (15) | 0.5621 (3) | 0.0098 (7) | |
Ow2 | 0.7191 (3) | 0.58570 (15) | 0.4683 (3) | 0.0105 (7) | |
Hw21 | 0.8439 (19) | 0.583 (2) | 0.557 (4) | 0.019 (10)* | |
H1 | 0.244 (5) | 0.764 (3) | 0.016 (6) | 0.053 (17)* | |
Hw11 | 0.686 (3) | 0.908 (3) | 0.468 (5) | 0.047 (15)* | |
Hw22 | 0.685 (7) | 0.5334 (19) | 0.401 (6) | 0.055 (16)* | |
Hw12 | 0.832 (7) | 0.961 (2) | 0.635 (6) | 0.060 (16)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Rb1 | 0.00794 (12) | 0.00754 (12) | 0.00307 (13) | −0.00039 (8) | 0.00087 (10) | 0.00014 (9) |
Rb2 | 0.00866 (13) | 0.00773 (13) | 0.00925 (14) | −0.00021 (9) | 0.00208 (10) | 0.00055 (10) |
P | 0.0060 (3) | 0.0052 (3) | 0.0022 (3) | 0.0000 (2) | 0.0012 (2) | 0.0003 (2) |
O1 | 0.0090 (9) | 0.0155 (10) | 0.0070 (10) | −0.0006 (7) | 0.0020 (8) | −0.0063 (8) |
O2 | 0.0089 (9) | 0.0088 (9) | 0.0083 (10) | −0.0003 (7) | 0.0039 (8) | 0.0026 (7) |
O3 | 0.0099 (9) | 0.0119 (9) | 0.0091 (10) | 0.0010 (7) | 0.0027 (8) | 0.0058 (8) |
O4 | 0.0091 (9) | 0.0095 (9) | 0.0072 (9) | 0.0003 (7) | 0.0037 (8) | −0.0029 (7) |
Ow1 | 0.0098 (9) | 0.0093 (10) | 0.0084 (10) | 0.0002 (7) | 0.0028 (8) | −0.0031 (7) |
Ow2 | 0.0092 (9) | 0.0105 (10) | 0.0102 (10) | −0.0001 (7) | 0.0031 (8) | −0.0036 (8) |
Rb1—O1i | 2.8753 (18) | Rb2—O3 | 3.497 (3) |
Rb1—O2ii | 3.158 (2) | Rb2—O3ii | 2.983 (2) |
Rb1—O3 | 2.8246 (18) | Rb2—O4 | 3.204 (2) |
Rb1—O3ii | 3.576 (3) | Rb2—O4vi | 3.522 (2) |
Rb1—O4iii | 3.154 (2) | Rb2—Ow1vii | 2.974 (2) |
Rb1—Ow1 | 2.977 (2) | Rb2—Ow1v | 3.178 (2) |
Rb1—Ow1ii | 2.943 (2) | Rb2—Ow2viii | 3.151 (2) |
Rb1—Ow2 | 2.946 (2) | Rb2—Ow2ii | 2.951 (2) |
Rb1—Ow2ii | 3.021 (2) | P—O1 | 1.595 (2) |
Rb2—O1iv | 3.395 (3) | P—O2 | 1.520 (2) |
Rb2—O1ii | 3.159 (2) | P—O3 | 1.525 (2) |
Rb2—O2iv | 3.470 (2) | P—O4 | 1.518 (2) |
Rb2—O2v | 3.130 (2) | ||
O1i—Rb1—O2ii | 133.50 (6) | O1ii—Rb2—Ow1v | 115.03 (6) |
O1i—Rb1—O3 | 149.97 (6) | O1ii—Rb2—Ow2viii | 153.46 (7) |
O1i—Rb1—O3ii | 113.10 (6) | O1ii—Rb2—Ow2ii | 103.22 (5) |
O1i—Rb1—O4iii | 68.96 (6) | O2iv—Rb2—O2v | 95.75 (5) |
O1i—Rb1—Ow1 | 81.59 (6) | O2iv—Rb2—O3 | 135.67 (4) |
O1i—Rb1—Ow1ii | 80.88 (6) | O2iv—Rb2—O3ii | 66.68 (5) |
O1i—Rb1—Ow2 | 120.10 (6) | O2iv—Rb2—O4 | 177.07 (5) |
O1i—Rb1—Ow2ii | 69.41 (6) | O2iv—Rb2—O4vi | 84.53 (5) |
O2ii—Rb1—O3 | 73.04 (6) | O2iv—Rb2—Ow1vii | 104.02 (6) |
O2ii—Rb1—O3ii | 43.10 (5) | O2iv—Rb2—Ow1v | 132.40 (5) |
O2ii—Rb1—O4iii | 100.18 (5) | O2iv—Rb2—Ow2viii | 47.89 (5) |
O2ii—Rb1—Ow1 | 143.51 (5) | O2iv—Rb2—Ow2ii | 69.30 (7) |
O2ii—Rb1—Ow1ii | 52.95 (5) | O2v—Rb2—O3 | 89.79 (6) |
O2ii—Rb1—Ow2 | 73.96 (7) | O2v—Rb2—O3ii | 126.14 (5) |
O2ii—Rb1—Ow2ii | 107.77 (7) | O2v—Rb2—O4 | 87.17 (5) |
O3—Rb1—O3ii | 75.21 (6) | O2v—Rb2—O4vi | 93.21 (5) |
O3—Rb1—O4iii | 127.21 (6) | O2v—Rb2—Ow1vii | 133.04 (5) |
O3—Rb1—Ow1 | 70.50 (6) | O2v—Rb2—Ow1v | 51.22 (5) |
O3—Rb1—Ow1ii | 125.40 (6) | O2v—Rb2—Ow2viii | 71.63 (7) |
O3—Rb1—Ow2 | 76.15 (6) | O2v—Rb2—Ow2ii | 52.68 (5) |
O3—Rb1—Ow2ii | 90.78 (6) | O3—Rb2—O3ii | 74.66 (6) |
O3ii—Rb1—O4iii | 134.24 (5) | O3—Rb2—O4 | 43.89 (5) |
O3ii—Rb1—Ow1 | 122.79 (6) | O3—Rb2—O4vi | 139.16 (4) |
O3ii—Rb1—Ow1ii | 60.95 (6) | O3—Rb2—Ow1vii | 103.75 (6) |
O3ii—Rb1—Ow2 | 115.87 (6) | O3—Rb2—Ow1v | 83.66 (6) |
O3ii—Rb1—Ow2ii | 64.68 (6) | O3—Rb2—Ow2viii | 161.31 (6) |
O4iii—Rb1—Ow1 | 102.94 (7) | O3—Rb2—Ow2ii | 79.97 (6) |
O4iii—Rb1—Ow1ii | 75.17 (7) | O3ii—Rb2—O4 | 111.36 (5) |
O4iii—Rb1—Ow2 | 52.48 (5) | O3ii—Rb2—O4vi | 131.72 (6) |
O4iii—Rb1—Ow2ii | 138.37 (5) | O3ii—Rb2—Ow1vii | 100.82 (6) |
Ow1—Rb1—Ow1ii | 161.79 (5) | O3ii—Rb2—Ow1v | 158.28 (7) |
Ow1—Rb1—Ow2 | 98.63 (7) | O3ii—Rb2—Ow2viii | 114.35 (6) |
Ow1—Rb1—Ow2ii | 71.41 (7) | O3ii—Rb2—Ow2ii | 73.73 (6) |
Ow1ii—Rb1—Ow2 | 94.40 (7) | O4—Rb2—O4vi | 95.56 (5) |
Ow1ii—Rb1—Ow2ii | 97.69 (7) | O4—Rb2—Ow1vii | 74.01 (7) |
Ow2—Rb1—Ow2ii | 165.84 (5) | O4—Rb2—Ow1v | 49.99 (5) |
O1iv—Rb2—O1ii | 76.16 (6) | O4—Rb2—Ow2viii | 133.78 (5) |
O1iv—Rb2—O2iv | 43.01 (4) | O4—Rb2—Ow2ii | 112.53 (7) |
O1iv—Rb2—O2v | 138.69 (5) | O4vi—Rb2—Ow1vii | 48.15 (5) |
O1iv—Rb2—O3 | 116.94 (5) | O4vi—Rb2—Ow1v | 67.28 (6) |
O1iv—Rb2—O3ii | 46.31 (6) | O4vi—Rb2—Ow2viii | 47.40 (4) |
O1iv—Rb2—O4 | 134.06 (5) | O4vi—Rb2—Ow2ii | 132.09 (5) |
O1iv—Rb2—O4vi | 86.10 (5) | Ow1vii—Rb2—Ow1v | 85.34 (6) |
O1iv—Rb2—Ow1vii | 73.47 (6) | Ow1vii—Rb2—Ow2viii | 90.92 (6) |
O1iv—Rb2—Ow1v | 153.11 (6) | Ow1vii—Rb2—Ow2ii | 172.54 (7) |
O1iv—Rb2—Ow2viii | 78.04 (6) | Ow1v—Rb2—Ow2viii | 86.11 (6) |
O1iv—Rb2—Ow2ii | 99.09 (6) | Ow1v—Rb2—Ow2ii | 101.60 (6) |
O1ii—Rb2—O2iv | 112.50 (5) | Ow2viii—Rb2—Ow2ii | 86.85 (6) |
O1ii—Rb2—O2v | 133.80 (7) | O1—P—O2 | 107.83 (13) |
O1ii—Rb2—O3 | 44.43 (6) | O1—P—O3 | 107.49 (11) |
O1ii—Rb2—O3ii | 48.27 (5) | O1—P—O4 | 104.77 (11) |
O1ii—Rb2—O4 | 65.05 (5) | O2—P—O3 | 110.61 (11) |
O1ii—Rb2—O4vi | 124.05 (5) | O3—P—O4 | 111.70 (14) |
O1ii—Rb2—Ow1vii | 75.90 (6) |
Symmetry codes: (i) x+1, y, z+1; (ii) x, −y+3/2, z+1/2; (iii) x+1, −y+3/2, z+1/2; (iv) x, y, z+1; (v) −x+1, −y+2, −z+1; (vi) −x, −y+2, −z+1; (vii) x−1, y, z; (viii) −x+1, y+1/2, −z+3/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O3ix | 0.97 (5) | 1.56 (5) | 2.536 (4) | 175 (3) |
Ow1—Hw11···O2 | 0.850 (19) | 1.88 (2) | 2.727 (2) | 171 (4) |
Ow1—Hw12···O4v | 0.85 (3) | 1.89 (3) | 2.697 (3) | 159 (5) |
Ow2—Hw21···O4iii | 0.850 (14) | 1.864 (17) | 2.704 (3) | 169 (3) |
Ow2—Hw22···O2x | 0.85 (3) | 1.86 (3) | 2.703 (3) | 171 (5) |
Symmetry codes: (iii) x+1, −y+3/2, z+1/2; (v) −x+1, −y+2, −z+1; (ix) x, −y+3/2, z−1/2; (x) −x+1, y−1/2, −z+1/2. |
Rb2HPO4.2H2O | Rb2HAsO4.2H2O | Cs2HPO4.2H2O | Cs2HAsO4.2H2O | ||
Actual structure | Disordered structure | d (Å) | d (Å) | d (Å) | d (Å) |
M1 (4 e 1) | M1 (4 e 2) | 0.063 | 0.055 | 0.053 | 0.056 |
M2 (4 e 1) | M2 (4 e 2) | 0.143 | 0.058 | 0.043 | 0.029 |
X (4 e 1) | X (4 e 2) | 0.130 | 0.057 | 0.068 | 0.065 |
O1/O3 (4 e 1) | O1 (8 f 2) | 0.173 | 0.120 | 0.082 | 0.089 |
O2/O4 (4 e 1) | O2 (8 f 2) | 0.126 | 0.059 | 0.045 | 0.034 |
Ow1/Ow2 (4 e 1) | Ow1 (8 f 2) | 0.116 | 0.052 | 0.031 | 0.025 |
Imax (h+k = 2n) | Iavg (h+k = 2n) | Imax (h+k = 2n+1) | Iavg (h+k = 2n+1) | Imax (h+k = 2n)/Imax(h+k = 2n+1) | |
Rb2HPO4.2H2O | 1000.0 | 39.0 | 64.1 | 6.1 | 15.6 |
Rb2HAsO4.2H2O | 1000.0 | 28.8 | 17.0 | 1.3 | 58.9 |
Cs2HPO4.2H2O | 1000.0 | 66.8 | 18.8 | 2.2 | 53.3 |
Cs2HAsO4.2H2O | 1000.0 | 52.9 | 15.9 | 1.7 | 63.0 |