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The four isotypic alkaline metal monohydrogen arsenate(V) and phosphate(V) dihydrates
M2H
XO
4·2H
2O (
M = Rb, Cs;
X = P, As) [namely dicaesium monohydrogen arsenate(V) dihydrate, Cs
2HAsO
4·2H
2O, dicaesium monohydrogen phosphate(V) dihydrate, Cs
2HPO
4·2H
2O, dirubidium monohydrogen arsenate(V) dihydrate, Rb
2HAsO
4·2H
2O, and dirubidium monohydrogen phosphate(V) dihydrate, Rb
2HPO
4·2H
2O] were synthesized by reaction of an aqueous H
3XO
4 solution with one equivalent of aqueous
M2CO
3. Their crystal structures are made up of undulating chains extending along [001] of tetrahedral [
XO
3(OH)]
− anions connected
via strong O—H
O hydrogen bonds. These chains are in turn connected into a three-dimensional network
via medium-strength hydrogen bonding involving the water molecules. Two crystallographically different
M+ cations are located in channels running along [001] or in the free space of the [
XO
3(OH)]
− chains, respectively. They are coordinated by eight and twelve O atoms forming irregular polyhedra. The structures possess pseudosymmetry. Due to the ordering of the protons in the [
XO
3(OH)]
− chains in the actual structures, the symmetry is reduced from
C2/
c to
P2
1/
c. Nevertheless, the deviation from
C2/
c symmetry is minute.
Supporting information
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) Dicaesium monohydrogen arsenate(V) dihydrate
top
Crystal data top
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 | |
Data collection top
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 top
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 | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | 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)* | |
Atomic displacement parameters (Å2) top | 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) |
Geometric parameters (Å, º) top
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. |
Hydrogen-bond geometry (Å, º) top
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) Dicaesium monohydrogen phosphate(V) dihydrate
top
Crystal data top
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 | |
Data collection top
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 top
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 | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | 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)* | |
Atomic displacement parameters (Å2) top | 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) |
Geometric parameters (Å, º) top
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. |
Hydrogen-bond geometry (Å, º) top
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) Dirubidium monohydrogen arsenate(V) dihydrate
top
Crystal data top
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 | |
Data collection top
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 top
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 | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | 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)* | |
Atomic displacement parameters (Å2) top | 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) |
Geometric parameters (Å, º) top
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. |
Hydrogen-bond geometry (Å, º) top
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) Dirubidium monohydrogen phosphate(V) dihydrate
top
Crystal data top
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 | |
Data collection top
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 top
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 | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | 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)* | |
Atomic displacement parameters (Å2) top | 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) |
Geometric parameters (Å, º) top
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. |
Hydrogen-bond geometry (Å, º) top
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. |
Distance d of the non-H atoms in the actual P21/c
structure of Rb2HPO4.2H2O to those in the hypothetical proton-disordered
C2/c structure. Multiplicity, Wyckoff positions and site symmetry
of atoms are indicated in parentheses. top | | 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 |
Maximum and average intensities of the reflections with
h+k = 2n and h+k = 2n+1 and ratio of
the maximum intensities of both classes. The maximum intensity value of each
data set was standardized to 1000.0 top | 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 |
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